# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Junk, Peter Courtney' 'Cole, Marcus L.' 'Evans, David J.' 'Louis, Lance M.' _publ_contact_author_name 'Peter C. Junk' _publ_contact_author_address ; School of Chemistry Monash University Box 23 Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email 'Peter.Junk@sci.monash.edu.au' _publ_contact_author_fax '61399054597' _publ_contact_author_phone '61399054570' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Structural and synthetic studies of magnesium and zinc tolylformamidinate complexes ; data_compound1.CIF _database_code_CSD 185261 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Mg N4 O2' _chemical_formula_weight 615.10 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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5039(6) _cell_length_b 16.3981(11) _cell_length_c 23.0294(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.339(2) _cell_angle_gamma 90.00 _cell_volume 3578.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9662 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16228 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.27 _reflns_number_total 5137 _reflns_number_gt 3425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.1867P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5137 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.003 _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 Mg1 Mg 0.50621(9) 0.36614(5) 0.23774(4) 0.0546(3) Uani 1 1 d . . . O1 O 0.6711(2) 0.38567(13) 0.18038(8) 0.0734(6) Uani 1 1 d . . . N1 N 0.4592(2) 0.25012(13) 0.19654(9) 0.0575(6) Uani 1 1 d . . . C1 C 0.3763(3) 0.20802(16) 0.15379(11) 0.0557(7) Uani 1 1 d . . . O2 O 0.3332(2) 0.34537(12) 0.29097(8) 0.0722(6) Uani 1 1 d . . . N2 N 0.6143(2) 0.26080(13) 0.27437(9) 0.0583(6) Uani 1 1 d . . . C2 C 0.3706(4) 0.1242(2) 0.14650(16) 0.0788(9) Uani 1 1 d . . . H2 H 0.418(3) 0.0930(17) 0.1720(13) 0.073(9) Uiso 1 1 d . . . N3 N 0.3951(2) 0.47374(13) 0.20398(9) 0.0606(6) Uani 1 1 d . . . C3 C 0.2877(4) 0.0903(3) 0.10094(18) 0.0907(11) Uani 1 1 d . . . H3 H 0.289(3) 0.041(2) 0.0978(14) 0.091(12) Uiso 1 1 d . . . N4 N 0.5552(2) 0.47982(13) 0.28118(10) 0.0609(6) Uani 1 1 d . . . C4 C 0.2074(3) 0.1344(2) 0.06128(14) 0.0769(9) Uani 1 1 d . . . C5 C 0.2086(4) 0.2167(2) 0.06977(15) 0.0822(10) Uani 1 1 d . . . H5 H 0.137(4) 0.249(2) 0.0470(15) 0.110(12) Uiso 1 1 d . . . C6 C 0.2909(3) 0.2526(2) 0.11466(14) 0.0750(9) Uani 1 1 d . . . H6 H 0.294(3) 0.3121(19) 0.1168(13) 0.083(9) Uiso 1 1 d . . . C7 C 0.1196(4) 0.0951(3) 0.01133(17) 0.1122(13) Uani 1 1 d . . . H7A H 0.1806 0.0679 -0.0138 0.168 Uiso 1 1 calc R . . H7B H 0.0664 0.1363 -0.0103 0.168 Uiso 1 1 calc R . . H7C H 0.0562 0.0563 0.0264 0.168 Uiso 1 1 calc R . . C8 C 0.7103(3) 0.22950(16) 0.31810(11) 0.0553(7) Uani 1 1 d . . . C9 C 0.7850(3) 0.1563(2) 0.31435(14) 0.0734(9) Uani 1 1 d . . . H9 H 0.781(3) 0.1264(18) 0.2792(14) 0.084(10) Uiso 1 1 d . . . C10 C 0.8731(3) 0.1299(2) 0.36107(15) 0.0800(9) Uani 1 1 d . . . H10 H 0.916(3) 0.0742(19) 0.3587(13) 0.093(10) Uiso 1 1 d . . . C11 C 0.8938(3) 0.1728(2) 0.41200(13) 0.0709(8) Uani 1 1 d . . . C12 C 0.8239(3) 0.2467(2) 0.41480(13) 0.0681(8) Uani 1 1 d . . . H12 H 0.837(3) 0.2848(18) 0.4458(13) 0.082(9) Uiso 1 1 d . . . C13 C 0.7336(3) 0.27351(18) 0.36921(13) 0.0623(7) Uani 1 1 d . . . H13 H 0.680(3) 0.3182(18) 0.3720(12) 0.076(9) Uiso 1 1 d . . . C14 C 0.9887(4) 0.1427(2) 0.46300(16) 0.1071(13) Uani 1 1 d . . . H14A H 1.0828 0.1624 0.4596 0.161 Uiso 1 1 calc R . . H14B H 0.9890 0.0842 0.4632 0.161 Uiso 1 1 calc R . . H14C H 0.9545 0.1624 0.4986 0.161 Uiso 1 1 calc R . . C15 C 0.5482(3) 0.21334(18) 0.23466(12) 0.0600(7) Uani 1 1 d . . . H15 H 0.559(3) 0.1494(18) 0.2370(11) 0.070(8) Uiso 1 1 d . . . C16 C 0.2919(3) 0.51191(16) 0.16616(12) 0.0582(7) Uani 1 1 d . . . C17 C 0.2768(3) 0.48941(17) 0.10803(13) 0.0624(7) Uani 1 1 d . . . H17 H 0.340(3) 0.4463(17) 0.0949(11) 0.072(8) Uiso 1 1 d . . . C18 C 0.1800(3) 0.52722(19) 0.06947(14) 0.0692(8) Uani 1 1 d . . . H18 H 0.175(3) 0.5118(16) 0.0315(13) 0.071(9) Uiso 1 1 d . . . C19 C 0.0944(3) 0.58887(19) 0.08616(13) 0.0723(8) Uani 1 1 d . . . C20 C 0.1072(4) 0.6098(2) 0.14431(16) 0.0888(11) Uani 1 1 d . . . H20 H 0.048(4) 0.650(2) 0.1574(15) 0.104(12) Uiso 1 1 d . . . C21 C 0.2022(3) 0.5724(2) 0.18374(15) 0.0779(9) Uani 1 1 d . . . H21 H 0.204(3) 0.5870(17) 0.2244(14) 0.084(9) Uiso 1 1 d . . . C22 C -0.0083(4) 0.6321(2) 0.04341(16) 0.1046(12) Uani 1 1 d . . . H22A H -0.0087 0.6060 0.0061 0.157 Uiso 1 1 calc R . . H22B H 0.0197 0.6880 0.0399 0.157 Uiso 1 1 calc R . . H22C H -0.1012 0.6298 0.0570 0.157 Uiso 1 1 calc R . . C23 C 0.6306(3) 0.52149(17) 0.32659(12) 0.0617(7) Uani 1 1 d . . . C24 C 0.5869(4) 0.5926(2) 0.35203(16) 0.0865(11) Uani 1 1 d . . . H24 H 0.507(4) 0.611(2) 0.3399(15) 0.095(13) Uiso 1 1 d . . . C25 C 0.6666(5) 0.6283(3) 0.39706(18) 0.0986(12) Uani 1 1 d . . . H25 H 0.631(4) 0.670(2) 0.4127(16) 0.104(13) Uiso 1 1 d . . . C26 C 0.7910(4) 0.5966(2) 0.42017(14) 0.0885(10) Uani 1 1 d . . . C27 C 0.8340(4) 0.5251(2) 0.39552(15) 0.0866(10) Uani 1 1 d . . . H27 H 0.925(4) 0.501(2) 0.4086(16) 0.114(13) Uiso 1 1 d . . . C28 C 0.7571(4) 0.4891(2) 0.34955(14) 0.0730(8) Uani 1 1 d . . . H28 H 0.793(3) 0.442(2) 0.3335(13) 0.089(10) Uiso 1 1 d . . . C29 C 0.8764(5) 0.6362(3) 0.47069(18) 0.1342(17) Uani 1 1 d . . . H29A H 0.9514 0.6677 0.4562 0.201 Uiso 1 1 calc R . . H29B H 0.9156 0.5948 0.4965 0.201 Uiso 1 1 calc R . . H29C H 0.8165 0.6713 0.4913 0.201 Uiso 1 1 calc R . . C30 C 0.4622(3) 0.51721(19) 0.24557(12) 0.0608(7) Uani 1 1 d . . . H30 H 0.448(2) 0.5775(17) 0.2492(10) 0.062(7) Uiso 1 1 d . . . C31 C 0.6591(5) 0.3697(4) 0.12026(17) 0.144(2) Uani 1 1 d . . . H31A H 0.5841 0.4023 0.1011 0.173 Uiso 1 1 calc R . . H31B H 0.6376 0.3126 0.1132 0.173 Uiso 1 1 calc R . . C32 C 0.7947(6) 0.3906(4) 0.0979(2) 0.169(2) Uani 1 1 d . . . H32A H 0.8210 0.3503 0.0698 0.203 Uiso 1 1 calc R . . H32B H 0.7898 0.4437 0.0792 0.203 Uiso 1 1 calc R . . C33 C 0.8923(5) 0.3916(5) 0.1466(3) 0.181(3) Uani 1 1 d . . . H33A H 0.9590 0.4359 0.1436 0.218 Uiso 1 1 calc R . . H33B H 0.9442 0.3406 0.1495 0.218 Uiso 1 1 calc R . . C34 C 0.8119(4) 0.4027(4) 0.1976(2) 0.1355(18) Uani 1 1 d . . . H34A H 0.8463 0.3661 0.2285 0.163 Uiso 1 1 calc R . . H34B H 0.8214 0.4583 0.2117 0.163 Uiso 1 1 calc R . . C35 C 0.1950(4) 0.3280(3) 0.26767(18) 0.1305(17) Uani 1 1 d . . . H35A H 0.1621 0.3711 0.2412 0.157 Uiso 1 1 calc R . . H35B H 0.1944 0.2772 0.2460 0.157 Uiso 1 1 calc R . . C36 C 0.1066(5) 0.3216(6) 0.3124(3) 0.207(3) Uani 1 1 d . . . H36A H 0.0575 0.2697 0.3100 0.249 Uiso 1 1 calc R . . H36B H 0.0370 0.3649 0.3094 0.249 Uiso 1 1 calc R . . C37 C 0.1897(6) 0.3275(4) 0.3661(2) 0.172(2) Uani 1 1 d . . . H37A H 0.1927 0.2754 0.3862 0.206 Uiso 1 1 calc R . . H37B H 0.1504 0.3679 0.3910 0.206 Uiso 1 1 calc R . . C38 C 0.3333(4) 0.3519(3) 0.35170(17) 0.1245(16) Uani 1 1 d . . . H38A H 0.3535 0.4074 0.3642 0.149 Uiso 1 1 calc R . . H38B H 0.4038 0.3161 0.3707 0.149 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0519(6) 0.0601(6) 0.0512(5) 0.0018(4) -0.0010(4) -0.0041(4) O1 0.0571(12) 0.1014(15) 0.0624(13) -0.0035(11) 0.0089(9) -0.0128(10) N1 0.0578(14) 0.0611(13) 0.0522(14) -0.0006(11) -0.0043(10) -0.0007(10) C1 0.0552(16) 0.0591(17) 0.0528(16) -0.0015(13) 0.0033(12) -0.0057(12) O2 0.0587(13) 0.0990(14) 0.0596(13) 0.0049(10) 0.0098(9) -0.0101(10) N2 0.0574(14) 0.0638(14) 0.0525(13) 0.0009(11) -0.0028(10) -0.0017(11) C2 0.091(3) 0.066(2) 0.076(2) -0.0045(18) -0.0132(19) 0.0027(17) N3 0.0596(14) 0.0615(14) 0.0592(14) 0.0039(11) -0.0055(11) -0.0041(11) C3 0.108(3) 0.064(2) 0.098(3) -0.019(2) -0.002(2) -0.009(2) N4 0.0576(14) 0.0655(14) 0.0582(14) -0.0001(11) -0.0045(11) -0.0079(11) C4 0.074(2) 0.088(2) 0.067(2) -0.0180(18) 0.0005(16) -0.0206(17) C5 0.080(2) 0.087(2) 0.076(2) 0.0013(18) -0.0204(18) -0.0066(18) C6 0.083(2) 0.0607(19) 0.077(2) 0.0002(16) -0.0201(17) -0.0088(15) C7 0.107(3) 0.131(3) 0.095(3) -0.038(2) -0.012(2) -0.031(2) C8 0.0479(15) 0.0631(16) 0.0544(16) 0.0033(13) 0.0005(12) -0.0024(12) C9 0.071(2) 0.085(2) 0.063(2) -0.0109(17) -0.0008(16) 0.0224(16) C10 0.077(2) 0.087(2) 0.074(2) -0.0041(18) -0.0056(17) 0.0288(17) C11 0.0606(19) 0.090(2) 0.0606(19) 0.0020(16) -0.0037(14) 0.0141(16) C12 0.0642(19) 0.081(2) 0.0574(19) -0.0083(16) -0.0063(14) 0.0026(15) C13 0.0581(18) 0.0609(18) 0.067(2) -0.0032(15) -0.0006(14) 0.0038(14) C14 0.105(3) 0.127(3) 0.084(3) -0.001(2) -0.027(2) 0.041(2) C15 0.0603(18) 0.0608(18) 0.0585(18) 0.0013(14) 0.0017(14) 0.0017(13) C16 0.0559(16) 0.0581(16) 0.0600(17) 0.0056(13) -0.0006(13) -0.0047(13) C17 0.0631(19) 0.0591(17) 0.0639(19) -0.0044(14) -0.0024(14) 0.0021(14) C18 0.071(2) 0.079(2) 0.056(2) -0.0033(16) -0.0048(15) 0.0003(16) C19 0.0637(19) 0.084(2) 0.068(2) 0.0040(16) -0.0036(15) 0.0122(16) C20 0.081(2) 0.110(3) 0.075(2) -0.008(2) 0.0025(18) 0.036(2) C21 0.074(2) 0.100(2) 0.059(2) -0.0046(18) 0.0033(16) 0.0229(18) C22 0.092(3) 0.128(3) 0.090(3) 0.007(2) -0.013(2) 0.039(2) C23 0.0616(18) 0.0681(18) 0.0552(17) -0.0005(14) 0.0024(13) -0.0169(14) C24 0.078(3) 0.097(3) 0.084(2) -0.025(2) -0.002(2) 0.006(2) C25 0.105(3) 0.102(3) 0.089(3) -0.038(2) 0.006(2) -0.009(2) C26 0.090(3) 0.112(3) 0.064(2) -0.015(2) 0.0010(18) -0.031(2) C27 0.082(3) 0.097(3) 0.078(2) -0.004(2) -0.0172(19) -0.019(2) C28 0.077(2) 0.070(2) 0.070(2) -0.0018(16) -0.0104(16) -0.0071(16) C29 0.138(4) 0.171(4) 0.090(3) -0.045(3) -0.017(3) -0.042(3) C30 0.0607(18) 0.0588(18) 0.0630(18) 0.0017(14) 0.0050(14) -0.0057(14) C31 0.109(3) 0.254(6) 0.071(3) -0.026(3) 0.019(2) -0.033(3) C32 0.118(4) 0.301(8) 0.093(4) 0.022(4) 0.041(3) -0.020(4) C33 0.088(4) 0.317(8) 0.145(5) -0.018(5) 0.047(4) -0.037(4) C34 0.075(3) 0.221(5) 0.111(3) -0.015(3) 0.015(2) -0.036(3) C35 0.064(2) 0.227(5) 0.100(3) 0.007(3) 0.006(2) -0.034(3) C36 0.075(3) 0.414(11) 0.135(5) 0.050(6) 0.023(3) -0.038(5) C37 0.130(4) 0.279(7) 0.116(4) 0.009(5) 0.070(4) -0.031(5) C38 0.106(3) 0.194(5) 0.076(3) -0.023(3) 0.024(2) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 2.149(2) . ? Mg1 N2 2.149(2) . ? Mg1 N4 2.150(2) . ? Mg1 O2 2.1510(19) . ? Mg1 N1 2.157(2) . ? Mg1 N3 2.170(2) . ? O1 C34 1.395(4) . ? O1 C31 1.405(4) . ? N1 C15 1.318(3) . ? N1 C1 1.396(3) . ? C1 C6 1.377(4) . ? C1 C2 1.384(4) . ? O2 C38 1.403(4) . ? O2 C35 1.410(4) . ? N2 C15 1.323(3) . ? N2 C8 1.404(3) . ? C2 C3 1.381(5) . ? N3 C30 1.319(3) . ? N3 C16 1.408(3) . ? C3 C4 1.355(5) . ? N4 C30 1.312(3) . ? N4 C23 1.400(3) . ? C4 C5 1.365(5) . ? C4 C7 1.513(4) . ? C5 C6 1.380(4) . ? C8 C13 1.384(4) . ? C8 C9 1.401(4) . ? C9 C10 1.382(4) . ? C10 C11 1.369(4) . ? C11 C12 1.386(4) . ? C11 C14 1.509(4) . ? C12 C13 1.377(4) . ? C16 C17 1.386(4) . ? C16 C21 1.389(4) . ? C17 C18 1.377(4) . ? C18 C19 1.371(4) . ? C19 C20 1.379(4) . ? C19 C22 1.509(4) . ? C20 C21 1.376(4) . ? C23 C28 1.381(4) . ? C23 C24 1.383(4) . ? C24 C25 1.369(5) . ? C25 C26 1.362(5) . ? C26 C27 1.379(5) . ? C26 C29 1.514(5) . ? C27 C28 1.373(4) . ? C31 C32 1.465(6) . ? C32 C33 1.402(6) . ? C33 C34 1.459(6) . ? C35 C36 1.381(6) . ? C36 C37 1.420(7) . ? C37 C38 1.484(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 N2 90.69(8) . . ? O1 Mg1 N4 90.82(8) . . ? N2 Mg1 N4 115.72(9) . . ? O1 Mg1 O2 176.82(8) . . ? N2 Mg1 O2 90.70(8) . . ? N4 Mg1 O2 91.15(9) . . ? O1 Mg1 N1 89.85(9) . . ? N2 Mg1 N1 62.67(8) . . ? N4 Mg1 N1 178.26(9) . . ? O2 Mg1 N1 88.24(9) . . ? O1 Mg1 N3 90.94(9) . . ? N2 Mg1 N3 177.87(9) . . ? N4 Mg1 N3 62.88(9) . . ? O2 Mg1 N3 87.74(8) . . ? N1 Mg1 N3 118.71(9) . . ? C34 O1 C31 108.8(3) . . ? C34 O1 Mg1 125.8(2) . . ? C31 O1 Mg1 124.7(2) . . ? C15 N1 C1 122.9(2) . . ? C15 N1 Mg1 90.55(17) . . ? C1 N1 Mg1 146.43(18) . . ? C6 C1 C2 115.6(3) . . ? C6 C1 N1 118.2(2) . . ? C2 C1 N1 126.2(3) . . ? C38 O2 C35 109.0(3) . . ? C38 O2 Mg1 127.8(2) . . ? C35 O2 Mg1 123.0(2) . . ? C15 N2 C8 122.0(2) . . ? C15 N2 Mg1 90.78(17) . . ? C8 N2 Mg1 147.21(18) . . ? C3 C2 C1 120.5(4) . . ? C30 N3 C16 119.0(2) . . ? C30 N3 Mg1 89.06(17) . . ? C16 N3 Mg1 151.69(18) . . ? C4 C3 C2 123.8(4) . . ? C30 N4 C23 121.4(3) . . ? C30 N4 Mg1 90.13(18) . . ? C23 N4 Mg1 148.4(2) . . ? C3 C4 C5 115.7(3) . . ? C3 C4 C7 122.4(3) . . ? C5 C4 C7 121.9(3) . . ? C4 C5 C6 121.8(3) . . ? C1 C6 C5 122.5(3) . . ? C13 C8 C9 116.7(3) . . ? C13 C8 N2 118.2(2) . . ? C9 C8 N2 125.0(3) . . ? C10 C9 C8 120.0(3) . . ? C11 C10 C9 123.0(3) . . ? C10 C11 C12 116.8(3) . . ? C10 C11 C14 122.5(3) . . ? C12 C11 C14 120.7(3) . . ? C13 C12 C11 121.1(3) . . ? C12 C13 C8 122.2(3) . . ? N1 C15 N2 116.0(3) . . ? C17 C16 C21 116.8(3) . . ? C17 C16 N3 119.7(2) . . ? C21 C16 N3 123.5(3) . . ? C18 C17 C16 121.3(3) . . ? C19 C18 C17 122.2(3) . . ? C18 C19 C20 116.5(3) . . ? C18 C19 C22 122.1(3) . . ? C20 C19 C22 121.4(3) . . ? C21 C20 C19 122.3(3) . . ? C20 C21 C16 120.9(3) . . ? C28 C23 C24 116.2(3) . . ? C28 C23 N4 118.7(3) . . ? C24 C23 N4 125.1(3) . . ? C25 C24 C23 121.0(4) . . ? C26 C25 C24 123.1(4) . . ? C25 C26 C27 116.1(3) . . ? C25 C26 C29 122.4(4) . . ? C27 C26 C29 121.5(4) . . ? C28 C27 C26 121.7(4) . . ? C27 C28 C23 121.8(4) . . ? N4 C30 N3 117.9(3) . . ? O1 C31 C32 107.2(4) . . ? C33 C32 C31 105.5(4) . . ? C32 C33 C34 106.9(4) . . ? O1 C34 C33 107.2(4) . . ? C36 C35 O2 109.5(4) . . ? C35 C36 C37 108.4(4) . . ? C36 C37 C38 106.5(4) . . ? O2 C38 C37 105.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.326 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.050 #===END data_compound2.CIF _database_code_CSD 185262 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Mg N4 O2' _chemical_formula_weight 615.10 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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-421c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 13.7728(19) _cell_length_b 13.7728(19) _cell_length_c 17.993(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3413.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.9821 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12878 _diffrn_reflns_av_R_equivalents 0.1598 _diffrn_reflns_av_sigmaI/netI 0.3125 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 28.38 _reflns_number_total 4221 _reflns_number_gt 1387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0780P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4221 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2590 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.004 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 Mg1 Mg 1.0000 0.5000 0.92519(10) 0.0333(4) Uani 1 2 d S . . N1B N 0.9176(2) 0.4969(2) 0.82230(14) 0.0308(7) Uani 1 1 d . . . N1A N 0.9177(2) 0.4972(3) 1.02719(15) 0.0336(7) Uani 1 1 d . . . O1 O 0.9948(2) 0.65483(17) 0.92546(15) 0.0371(6) Uani 1 1 d . . . C8B C 1.0000 0.5000 0.7853(3) 0.0320(13) Uani 1 2 d S . . H8B H 1.0000 0.5000 0.7325 0.038 Uiso 1 2 calc SR . . C8A C 1.0000 0.5000 1.0648(3) 0.0350(13) Uani 1 2 d S . . H8A H 1.0000 0.5000 1.1176 0.042 Uiso 1 2 calc SR . . C1A C 0.8307(3) 0.4815(3) 1.0666(2) 0.0377(12) Uani 1 1 d . . . C2B C 0.8221(3) 0.5754(3) 0.7253(2) 0.0398(11) Uani 1 1 d . . . H2B H 0.8747 0.6180 0.7152 0.048 Uiso 1 1 calc R . . C1B C 0.8313(3) 0.5061(3) 0.7813(2) 0.0310(9) Uani 1 1 d . . . C3A C 0.7390(4) 0.3992(3) 1.1625(2) 0.0545(14) Uani 1 1 d . . . H3A H 0.7370 0.3553 1.2032 0.065 Uiso 1 1 calc R . . C4B C 0.6597(3) 0.5230(3) 0.6995(2) 0.0430(12) Uani 1 1 d . . . H4B H 0.6008 0.5287 0.6724 0.052 Uiso 1 1 calc R . . C1 C 0.9485(3) 0.7153(3) 0.8696(2) 0.0474(13) Uani 1 1 d . . . H1A H 0.8856 0.6870 0.8540 0.057 Uiso 1 1 calc R . . H1B H 0.9906 0.7223 0.8253 0.057 Uiso 1 1 calc R . . C2A C 0.8254(3) 0.4147(3) 1.1244(2) 0.0456(11) Uani 1 1 d . . . H2A H 0.8817 0.3791 1.1381 0.055 Uiso 1 1 calc R . . C7A C 0.7516(3) 0.6044(3) 0.9844(2) 0.0509(13) Uani 1 1 d . . . H7A1 H 0.8048 0.6496 0.9947 0.076 Uiso 1 1 calc R . . H7A2 H 0.6901 0.6401 0.9826 0.076 Uiso 1 1 calc R . . H7A3 H 0.7629 0.5724 0.9365 0.076 Uiso 1 1 calc R . . C3 C 1.0184(3) 0.8185(3) 0.9596(3) 0.0531(14) Uani 1 1 d . . . H3B H 1.0774 0.8414 0.9337 0.064 Uiso 1 1 calc R . . H3C H 1.0040 0.8627 1.0016 0.064 Uiso 1 1 calc R . . C7B C 0.7621(3) 0.3679(3) 0.8567(2) 0.0450(12) Uani 1 1 d . . . H7B1 H 0.7051 0.3253 0.8551 0.068 Uiso 1 1 calc R . . H7B2 H 0.7660 0.3992 0.9055 0.068 Uiso 1 1 calc R . . H7B3 H 0.8209 0.3294 0.8482 0.068 Uiso 1 1 calc R . . C6B C 0.7535(3) 0.4440(3) 0.7975(2) 0.0373(11) Uani 1 1 d . . . C4 C 1.0298(3) 0.7158(3) 0.9857(2) 0.0406(12) Uani 1 1 d . . . H4A H 1.0988 0.7015 0.9966 0.049 Uiso 1 1 calc R . . H4C H 0.9913 0.7046 1.0314 0.049 Uiso 1 1 calc R . . C2 C 0.9336(4) 0.8116(3) 0.9072(3) 0.0610(16) Uani 1 1 d . . . H2C H 0.8712 0.8130 0.9345 0.073 Uiso 1 1 calc R . . H2D H 0.9345 0.8654 0.8706 0.073 Uiso 1 1 calc R . . C5B C 0.6687(3) 0.4534(3) 0.7555(2) 0.0427(13) Uani 1 1 d . . . H5B H 0.6156 0.4113 0.7653 0.051 Uiso 1 1 calc R . . C5A C 0.6617(3) 0.5121(4) 1.0817(3) 0.0530(13) Uani 1 1 d . . . H5A H 0.6045 0.5452 1.0666 0.064 Uiso 1 1 calc R . . C3B C 0.7365(3) 0.5829(3) 0.6838(2) 0.0420(11) Uani 1 1 d . . . H3B1 H 0.7316 0.6294 0.6450 0.050 Uiso 1 1 calc R . . C6A C 0.7471(4) 0.5297(3) 1.0443(2) 0.0421(12) Uani 1 1 d . . . C4A C 0.6565(4) 0.4476(4) 1.1409(3) 0.0611(15) Uani 1 1 d . . . H4A1 H 0.5967 0.4370 1.1660 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0387(10) 0.0364(10) 0.0246(10) 0.000 0.000 -0.0023(12) N1B 0.0357(18) 0.0381(18) 0.0186(16) 0.0014(19) -0.0012(17) -0.002(2) N1A 0.0318(19) 0.0458(19) 0.0234(17) -0.002(2) 0.0004(17) -0.005(2) O1 0.0506(16) 0.0336(15) 0.0271(14) 0.0010(15) -0.0033(16) 0.0042(18) C8B 0.050(4) 0.032(3) 0.014(3) 0.000 0.000 0.010(4) C8A 0.051(4) 0.036(3) 0.018(3) 0.000 0.000 -0.001(4) C1A 0.044(3) 0.043(3) 0.026(3) -0.006(2) 0.001(2) -0.006(2) C2B 0.047(3) 0.038(3) 0.034(3) -0.005(2) -0.001(2) 0.000(2) C1B 0.031(3) 0.035(2) 0.027(2) 0.003(3) -0.003(2) 0.004(2) C3A 0.069(4) 0.059(3) 0.036(3) -0.005(2) 0.019(3) -0.021(3) C4B 0.049(3) 0.040(3) 0.039(3) -0.006(2) -0.013(2) 0.009(2) C1 0.070(3) 0.039(3) 0.033(3) -0.001(2) -0.012(2) 0.010(2) C2A 0.055(3) 0.048(3) 0.034(3) -0.008(3) 0.001(2) -0.005(2) C7A 0.039(3) 0.062(3) 0.052(3) -0.009(3) -0.006(3) 0.009(2) C3 0.061(4) 0.045(3) 0.054(3) -0.006(3) 0.001(3) 0.000(3) C7B 0.050(3) 0.043(3) 0.043(3) 0.003(2) 0.002(2) -0.005(2) C6B 0.043(3) 0.038(3) 0.031(3) -0.009(2) -0.005(2) 0.008(2) C4 0.054(3) 0.033(3) 0.034(3) -0.006(2) 0.000(2) 0.000(2) C2 0.080(4) 0.038(3) 0.065(4) -0.009(3) -0.032(3) 0.005(3) C5B 0.040(3) 0.042(3) 0.046(3) -0.012(2) -0.002(3) -0.003(2) C5A 0.037(3) 0.061(4) 0.062(3) -0.016(3) 0.012(3) -0.003(3) C3B 0.049(3) 0.047(3) 0.030(3) 0.005(2) -0.007(2) -0.002(2) C6A 0.049(3) 0.040(3) 0.037(3) -0.012(2) 0.005(3) -0.004(2) C4A 0.046(3) 0.071(4) 0.066(4) -0.022(3) 0.028(3) -0.017(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 Mg1 O1 2.134(2) 3_765 ? Mg1 O1 2.134(2) . ? Mg1 N1A 2.158(3) 3_765 ? Mg1 N1A 2.158(3) . ? Mg1 N1B 2.172(3) . ? Mg1 N1B 2.172(3) 3_765 ? N1B C8B 1.316(4) . ? N1B C1B 1.404(4) . ? N1A C8A 1.321(4) . ? N1A C1A 1.409(5) . ? O1 C4 1.454(4) . ? O1 C1 1.453(5) . ? C8B N1B 1.316(4) 3_765 ? C8B H8B 0.9500 . ? C8A N1A 1.321(4) 3_765 ? C8A H8A 0.9500 . ? C1A C2A 1.390(6) . ? C1A C6A 1.388(6) . ? C2B C1B 1.393(6) . ? C2B C3B 1.400(5) . ? C2B H2B 0.9500 . ? C1B C6B 1.402(5) . ? C3A C4A 1.374(6) . ? C3A C2A 1.389(6) . ? C3A H3A 0.9500 . ? C4B C3B 1.370(5) . ? C4B C5B 1.396(5) . ? C4B H4B 0.9500 . ? C1 C2 1.504(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2A H2A 0.9500 . ? C7A C6A 1.492(5) . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C3 C4 1.498(5) . ? C3 C2 1.505(6) . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C7B C6B 1.499(5) . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C6B C5B 1.398(5) . ? C4 H4A 0.9900 . ? C4 H4C 0.9900 . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C5B H5B 0.9500 . ? C5A C6A 1.376(6) . ? C5A C4A 1.388(6) . ? C5A H5A 0.9500 . ? C3B H3B1 0.9500 . ? C4A H4A1 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 O1 179.74(19) 3_765 . ? O1 Mg1 N1A 89.93(13) 3_765 3_765 ? O1 Mg1 N1A 89.85(13) . 3_765 ? O1 Mg1 N1A 89.85(13) 3_765 . ? O1 Mg1 N1A 89.93(13) . . ? N1A Mg1 N1A 63.43(17) 3_765 . ? O1 Mg1 N1B 90.00(13) 3_765 . ? O1 Mg1 N1B 90.22(13) . . ? N1A Mg1 N1B 179.81(14) 3_765 . ? N1A Mg1 N1B 116.75(10) . . ? O1 Mg1 N1B 90.22(13) 3_765 3_765 ? O1 Mg1 N1B 90.00(13) . 3_765 ? N1A Mg1 N1B 116.75(10) 3_765 3_765 ? N1A Mg1 N1B 179.81(14) . 3_765 ? N1B Mg1 N1B 63.07(16) . 3_765 ? C8B N1B C1B 117.5(3) . . ? C8B N1B Mg1 88.8(3) . . ? C1B N1B Mg1 152.7(3) . . ? C8A N1A C1A 118.4(3) . . ? C8A N1A Mg1 89.1(3) . . ? C1A N1A Mg1 151.4(3) . . ? C4 O1 C1 109.3(3) . . ? C4 O1 Mg1 124.6(2) . . ? C1 O1 Mg1 125.8(2) . . ? N1B C8B N1B 119.3(5) 3_765 . ? N1B C8B H8B 120.3 3_765 . ? N1B C8B H8B 120.3 . . ? N1A C8A N1A 118.3(5) . 3_765 ? N1A C8A H8A 120.9 . . ? N1A C8A H8A 120.9 3_765 . ? C2A C1A C6A 119.3(4) . . ? C2A C1A N1A 121.5(4) . . ? C6A C1A N1A 119.1(4) . . ? C1B C2B C3B 120.9(4) . . ? C1B C2B H2B 119.5 . . ? C3B C2B H2B 119.5 . . ? C2B C1B N1B 121.2(4) . . ? C2B C1B C6B 119.9(4) . . ? N1B C1B C6B 118.9(4) . . ? C4A C3A C2A 119.6(4) . . ? C4A C3A H3A 120.2 . . ? C2A C3A H3A 120.2 . . ? C3B C4B C5B 119.6(4) . . ? C3B C4B H4B 120.2 . . ? C5B C4B H4B 120.2 . . ? O1 C1 C2 104.7(3) . . ? O1 C1 H1A 110.8 . . ? C2 C1 H1A 110.8 . . ? O1 C1 H1B 110.8 . . ? C2 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? C3A C2A C1A 121.0(4) . . ? C3A C2A H2A 119.5 . . ? C1A C2A H2A 119.5 . . ? C6A C7A H7A1 109.5 . . ? C6A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C6A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C4 C3 C2 102.7(4) . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? C4 C3 H3C 111.2 . . ? C2 C3 H3C 111.2 . . ? H3B C3 H3C 109.1 . . ? C6B C7B H7B1 109.5 . . ? C6B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C6B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C5B C6B C1B 118.0(4) . . ? C5B C6B C7B 121.0(4) . . ? C1B C6B C7B 120.9(4) . . ? O1 C4 C3 106.0(3) . . ? O1 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? O1 C4 H4C 110.5 . . ? C3 C4 H4C 110.5 . . ? H4A C4 H4C 108.7 . . ? C1 C2 C3 103.4(4) . . ? C1 C2 H2C 111.1 . . ? C3 C2 H2C 111.1 . . ? C1 C2 H2D 111.1 . . ? C3 C2 H2D 111.1 . . ? H2C C2 H2D 109.1 . . ? C6B C5B C4B 121.9(4) . . ? C6B C5B H5B 119.1 . . ? C4B C5B H5B 119.1 . . ? C6A C5A C4A 122.1(5) . . ? C6A C5A H5A 118.9 . . ? C4A C5A H5A 118.9 . . ? C4B C3B C2B 119.7(4) . . ? C4B C3B H3B1 120.2 . . ? C2B C3B H3B1 120.2 . . ? C5A C6A C1A 118.9(4) . . ? C5A C6A C7A 120.7(5) . . ? C1A C6A C7A 120.3(4) . . ? C3A C4A C5A 119.0(4) . . ? C3A C4A H4A1 120.5 . . ? C5A C4A H4A1 120.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.249 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.049 #===END data_compound3.CIF _database_code_CSD 185263 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Mg N4 O4' _chemical_formula_weight 651.13 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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 10.125(9) _cell_length_b 22.47(2) _cell_length_c 8.326(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1894(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9755 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8363 _diffrn_reflns_av_R_equivalents 0.1500 _diffrn_reflns_av_sigmaI/netI 0.1244 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2707 _reflns_number_gt 1362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.6(8) _refine_ls_number_reflns 2707 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1926 _refine_ls_wR_factor_gt 0.1549 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _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 Mg1 Mg 1.0000 1.0000 1.4214(3) 0.0679(8) Uani 1 2 d S . . O1 O 1.0519(4) 0.9466(2) 1.6235(5) 0.0927(14) Uani 1 1 d . . . N1 N 1.1271(5) 0.9531(2) 1.2632(5) 0.0686(13) Uani 1 1 d . . . C1 C 1.1400(6) 0.9026(3) 1.1632(6) 0.0641(15) Uani 1 1 d . . . O2 O 1.3874(7) 1.0358(3) 0.9474(6) 0.161(3) Uani 1 1 d . . . N2 N 1.1935(4) 1.0356(2) 1.3833(5) 0.0661(12) Uani 1 1 d . . . C2 C 1.2537(6) 0.8851(3) 1.0901(7) 0.0790(17) Uani 1 1 d . . . H2 H 1.3301 0.9077 1.1025 0.095 Uiso 1 1 calc R . . C3 C 1.2566(8) 0.8338(3) 0.9969(9) 0.092(2) Uani 1 1 d . . . H3 H 1.3356 0.8227 0.9485 0.111 Uiso 1 1 calc R . . C4 C 1.1481(8) 0.7994(3) 0.9742(8) 0.0842(19) Uani 1 1 d . . . C5 C 1.0356(8) 0.8172(3) 1.0475(9) 0.102(3) Uani 1 1 d . . . H5 H 0.9594 0.7945 1.0350 0.123 Uiso 1 1 calc R . . C6 C 1.0306(7) 0.8682(3) 1.1406(8) 0.092(2) Uani 1 1 d . . . H6 H 0.9513 0.8791 1.1886 0.111 Uiso 1 1 calc R . . C7 C 1.1502(8) 0.7442(3) 0.8679(11) 0.132(3) Uani 1 1 d . . . H7A H 1.2308 0.7226 0.8855 0.198 Uiso 1 1 calc R . . H7B H 1.1448 0.7559 0.7572 0.198 Uiso 1 1 calc R . . H7C H 1.0763 0.7192 0.8939 0.198 Uiso 1 1 calc R . . C8 C 1.2867(6) 1.0799(2) 1.4184(6) 0.0607(14) Uani 1 1 d . . . C9 C 1.4133(6) 1.0810(3) 1.3751(7) 0.0840(19) Uani 1 1 d . . . H9 H 1.4463 1.0499 1.3130 0.101 Uiso 1 1 calc R . . C10 C 1.4974(7) 1.1266(3) 1.4194(8) 0.098(2) Uani 1 1 d . . . H10 H 1.5851 1.1257 1.3863 0.118 Uiso 1 1 calc R . . C11 C 1.4545(8) 1.1724(3) 1.5095(9) 0.086(2) Uani 1 1 d . . . C12 C 1.3254(8) 1.1721(3) 1.5552(8) 0.087(2) Uani 1 1 d . . . H12 H 1.2929 1.2034 1.6167 0.104 Uiso 1 1 calc R . . C13 C 1.2428(7) 1.1270(3) 1.5129(8) 0.0804(18) Uani 1 1 d . . . H13 H 1.1555 1.1277 1.5477 0.096 Uiso 1 1 calc R . . C14 C 1.5465(8) 1.2221(3) 1.5577(11) 0.137(3) Uani 1 1 d . . . H14A H 1.5564 1.2494 1.4698 0.205 Uiso 1 1 calc R . . H14B H 1.6312 1.2058 1.5854 0.205 Uiso 1 1 calc R . . H14C H 1.5106 1.2427 1.6488 0.205 Uiso 1 1 calc R . . C15 C 1.2212(7) 0.9923(3) 1.2805(7) 0.0670(16) Uani 1 1 d . . . H15 H 1.308(5) 0.990(2) 1.246(6) 0.070(19) Uiso 1 1 d . . . C16 C 1.0568(8) 0.9789(4) 1.7672(7) 0.140(4) Uani 1 1 d . . . H16A H 1.1394 1.0006 1.7745 0.168 Uiso 1 1 calc R . . H16B H 1.0508 0.9522 1.8584 0.168 Uiso 1 1 calc R . . C17 C 1.1476(9) 0.9002(4) 1.6184(10) 0.133(3) Uani 1 1 d . . . H17A H 1.1208 0.8684 1.6883 0.199 Uiso 1 1 calc R . . H17B H 1.2315 0.9154 1.6529 0.199 Uiso 1 1 calc R . . H17C H 1.1550 0.8855 1.5105 0.199 Uiso 1 1 calc R . . C18 C 1.4692(11) 1.0285(4) 0.8212(9) 0.145(4) Uani 1 1 d . . . H18A H 1.5367 1.0591 0.8239 0.174 Uiso 1 1 calc R . . H18B H 1.4194 1.0333 0.7224 0.174 Uiso 1 1 calc R . . C19 C 1.3245(14) 1.0901(4) 0.9581(12) 0.208(6) Uani 1 1 d . . . H19A H 1.2342 1.0841 0.9894 0.312 Uiso 1 1 calc R . . H19B H 1.3273 1.1097 0.8556 0.312 Uiso 1 1 calc R . . H19C H 1.3682 1.1144 1.0368 0.312 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0836(18) 0.0759(18) 0.0443(15) 0.000 0.000 0.0026(15) O1 0.115(4) 0.112(4) 0.051(2) 0.015(3) -0.015(2) -0.008(3) N1 0.078(3) 0.074(4) 0.054(3) -0.005(3) 0.003(2) -0.003(3) C1 0.066(4) 0.075(4) 0.051(3) 0.009(3) 0.004(3) 0.000(4) O2 0.266(7) 0.146(5) 0.070(3) 0.007(4) 0.051(4) 0.015(5) N2 0.081(3) 0.069(3) 0.049(3) -0.007(3) -0.005(2) 0.004(3) C2 0.084(5) 0.080(4) 0.074(4) -0.002(4) -0.009(4) -0.002(4) C3 0.105(6) 0.087(5) 0.085(5) -0.011(4) 0.001(4) 0.004(5) C4 0.119(6) 0.064(4) 0.070(5) 0.004(3) 0.008(4) -0.005(4) C5 0.120(7) 0.081(5) 0.106(6) -0.016(4) 0.025(5) -0.030(4) C6 0.104(6) 0.086(5) 0.086(5) -0.009(4) 0.020(4) -0.015(4) C7 0.187(8) 0.079(5) 0.130(7) -0.030(5) 0.012(6) -0.014(5) C8 0.073(4) 0.067(4) 0.042(3) 0.003(3) -0.008(3) -0.002(3) C9 0.071(5) 0.094(5) 0.087(5) -0.020(4) 0.004(4) -0.013(4) C10 0.083(4) 0.115(6) 0.098(5) -0.012(5) 0.003(5) -0.014(5) C11 0.106(6) 0.078(5) 0.075(5) 0.010(4) -0.019(4) -0.016(4) C12 0.111(6) 0.071(5) 0.079(5) 0.001(4) -0.013(4) -0.006(4) C13 0.088(5) 0.074(4) 0.079(4) -0.004(4) -0.004(4) 0.005(4) C14 0.171(9) 0.108(6) 0.132(7) 0.002(6) -0.034(6) -0.057(6) C15 0.071(5) 0.076(5) 0.054(4) 0.007(3) -0.001(3) -0.003(4) C16 0.191(11) 0.189(12) 0.041(3) 0.007(5) -0.022(4) -0.016(7) C17 0.164(8) 0.132(7) 0.103(6) 0.031(6) -0.022(6) 0.025(6) C18 0.182(11) 0.184(11) 0.069(4) 0.013(5) 0.008(6) -0.036(9) C19 0.396(19) 0.119(8) 0.110(7) 0.004(7) -0.013(9) 0.064(11) _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 Mg1 N1 2.121(5) 2_775 ? Mg1 N1 2.121(5) . ? Mg1 O1 2.133(5) 2_775 ? Mg1 O1 2.133(5) . ? Mg1 N2 2.140(5) 2_775 ? Mg1 N2 2.140(5) . ? Mg1 C15 2.534(8) 2_775 ? O1 C16 1.401(8) . ? O1 C17 1.424(8) . ? N1 C15 1.305(7) . ? N1 C1 1.413(7) . ? C1 C2 1.360(8) . ? C1 C6 1.364(8) . ? O2 C18 1.348(9) . ? O2 C19 1.378(10) . ? N2 C15 1.326(7) . ? N2 C8 1.402(7) . ? C2 C3 1.389(8) . ? C3 C4 1.357(9) . ? C4 C5 1.352(9) . ? C4 C7 1.524(8) . ? C5 C6 1.384(8) . ? C8 C9 1.332(7) . ? C8 C13 1.392(7) . ? C9 C10 1.383(8) . ? C10 C11 1.346(8) . ? C11 C12 1.362(9) . ? C11 C14 1.508(8) . ? C12 C13 1.359(8) . ? C16 C16 1.490(15) 2_775 ? C18 C18 1.424(16) 2_875 ? 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 N1 Mg1 N1 103.2(3) 2_775 . ? N1 Mg1 O1 93.51(18) 2_775 2_775 ? N1 Mg1 O1 156.76(18) . 2_775 ? N1 Mg1 O1 156.76(18) 2_775 . ? N1 Mg1 O1 93.51(18) . . ? O1 Mg1 O1 75.8(3) 2_775 . ? N1 Mg1 N2 62.49(19) 2_775 2_775 ? N1 Mg1 N2 106.1(2) . 2_775 ? O1 Mg1 N2 95.83(18) 2_775 2_775 ? O1 Mg1 N2 97.61(18) . 2_775 ? N1 Mg1 N2 106.1(2) 2_775 . ? N1 Mg1 N2 62.49(19) . . ? O1 Mg1 N2 97.61(18) 2_775 . ? O1 Mg1 N2 95.83(18) . . ? N2 Mg1 N2 162.9(3) 2_775 . ? N1 Mg1 C15 30.97(17) 2_775 2_775 ? N1 Mg1 C15 106.4(2) . 2_775 ? O1 Mg1 C15 96.25(18) 2_775 2_775 ? O1 Mg1 C15 128.43(19) . 2_775 ? N2 Mg1 C15 31.54(18) 2_775 2_775 ? N2 Mg1 C15 135.6(2) . 2_775 ? C16 O1 C17 112.4(5) . . ? C16 O1 Mg1 113.0(4) . . ? C17 O1 Mg1 123.8(4) . . ? C15 N1 C1 122.6(5) . . ? C15 N1 Mg1 92.3(4) . . ? C1 N1 Mg1 145.2(4) . . ? C2 C1 C6 117.5(6) . . ? C2 C1 N1 125.0(6) . . ? C6 C1 N1 117.5(6) . . ? C18 O2 C19 116.3(8) . . ? C15 N2 C8 120.9(5) . . ? C15 N2 Mg1 90.9(4) . . ? C8 N2 Mg1 148.2(4) . . ? C1 C2 C3 120.5(6) . . ? C4 C3 C2 122.3(7) . . ? C5 C4 C3 116.8(6) . . ? C5 C4 C7 120.9(7) . . ? C3 C4 C7 122.3(7) . . ? C4 C5 C6 121.8(7) . . ? C1 C6 C5 121.2(7) . . ? C9 C8 C13 116.5(6) . . ? C9 C8 N2 127.1(6) . . ? C13 C8 N2 116.3(6) . . ? C8 C9 C10 122.3(7) . . ? C11 C10 C9 121.1(7) . . ? C10 C11 C12 117.5(7) . . ? C10 C11 C14 121.0(8) . . ? C12 C11 C14 121.5(7) . . ? C13 C12 C11 121.5(7) . . ? C12 C13 C8 121.1(6) . . ? N1 C15 N2 114.3(6) . . ? O1 C16 C16 107.6(5) . 2_775 ? O2 C18 C18 112.3(8) . 2_875 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.224 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.040 #===END data_compound4.CIF _database_code_CSD 185264 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 Mg N6' _chemical_formula_weight 587.10 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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.519(7) _cell_length_b 14.559(8) _cell_length_c 18.815(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.055(7) _cell_angle_gamma 90.00 _cell_volume 3456(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9672 _exptl_absorpt_correction_T_max 0.9712 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14959 _diffrn_reflns_av_R_equivalents 0.1738 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.37 _reflns_number_total 4973 _reflns_number_gt 2753 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1404P)^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 SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 4973 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1407 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2586 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.014 _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 Mg1 Mg 0.56079(11) 0.64421(9) 0.19577(8) 0.0464(5) Uani 1 1 d . . . N1 N 0.4433(3) 0.5562(2) 0.10973(19) 0.0467(9) Uani 1 1 d . . . C1 C 0.3400(3) 0.5345(3) 0.0602(2) 0.0468(11) Uani 1 1 d . . . N2 N 0.6054(3) 0.5058(2) 0.1814(2) 0.0475(9) Uani 1 1 d . . . C2 C 0.2829(4) 0.4605(3) 0.0715(3) 0.0572(13) Uani 1 1 d . . . H2 H 0.305(3) 0.422(3) 0.114(2) 0.048(12) Uiso 1 1 d . . . N3 N 0.5096(3) 0.6241(2) 0.2921(2) 0.0533(10) Uani 1 1 d . . . C3 C 0.1835(4) 0.4394(4) 0.0204(3) 0.0620(14) Uani 1 1 d . . . H3 H 0.138(3) 0.391(3) 0.028(2) 0.044(11) Uiso 1 1 d . . . N4 N 0.6753(3) 0.6728(3) 0.3135(2) 0.0560(10) Uani 1 1 d . . . C4 C 0.1373(4) 0.4929(4) -0.0435(3) 0.0592(13) Uani 1 1 d . . . N5 N 0.4850(3) 0.7839(2) 0.1681(2) 0.0534(10) Uani 1 1 d . . . C5 C 0.1939(4) 0.5669(3) -0.0542(3) 0.0607(13) Uani 1 1 d . . . H5 H 0.1641 0.6035 -0.0972 0.073 Uiso 1 1 calc R . . N6 N 0.6453(3) 0.7006(2) 0.1189(2) 0.0529(10) Uani 1 1 d . . . C6 C 0.2930(4) 0.5883(3) -0.0033(3) 0.0531(12) Uani 1 1 d . . . H6 H 0.3286 0.6394 -0.0117 0.064 Uiso 1 1 calc R . . C7 C 0.0296(4) 0.4704(4) -0.0999(3) 0.0859(18) Uani 1 1 d . . . H7A H -0.0156 0.5232 -0.1073 0.129 Uiso 1 1 calc R . . H7B H -0.0001 0.4204 -0.0811 0.129 Uiso 1 1 calc R . . H7C H 0.0353 0.4533 -0.1476 0.129 Uiso 1 1 calc R . . C8 C 0.6847(3) 0.4403(3) 0.2040(2) 0.0476(11) Uani 1 1 d . . . C9 C 0.6784(4) 0.3509(3) 0.1759(3) 0.0550(12) Uani 1 1 d . . . H9 H 0.618(4) 0.335(3) 0.141(2) 0.048(13) Uiso 1 1 d . . . C10 C 0.7624(4) 0.2908(3) 0.2015(3) 0.0681(15) Uani 1 1 d . . . H10 H 0.7552 0.2317 0.1814 0.082 Uiso 1 1 calc R . . C11 C 0.8566(4) 0.3166(4) 0.2561(3) 0.0729(16) Uani 1 1 d . . . C12 C 0.8628(4) 0.4041(4) 0.2846(3) 0.0785(16) Uani 1 1 d . . . H12 H 0.9254 0.4232 0.3223 0.094 Uiso 1 1 calc R . . C13 C 0.7788(4) 0.4647(4) 0.2588(3) 0.0646(15) Uani 1 1 d . . . H13 H 0.788(3) 0.520(3) 0.282(2) 0.048(13) Uiso 1 1 d . . . C14 C 0.9500(5) 0.2513(4) 0.2833(4) 0.109(2) Uani 1 1 d . . . H14A H 0.9782 0.2503 0.3380 0.164 Uiso 1 1 calc R . . H14B H 1.0039 0.2715 0.2648 0.164 Uiso 1 1 calc R . . H14C H 0.9271 0.1907 0.2645 0.164 Uiso 1 1 calc R . . C15 C 0.5116(4) 0.4878(3) 0.1319(2) 0.0454(11) Uani 1 1 d . . . H15 H 0.491(3) 0.425(3) 0.1066(19) 0.034(10) Uiso 1 1 d . . . C16 C 0.4270(4) 0.5953(3) 0.3156(3) 0.0521(12) Uani 1 1 d . . . C17 C 0.3363(4) 0.5632(3) 0.2611(3) 0.0579(13) Uani 1 1 d . . . H17 H 0.3314 0.5627 0.2105 0.070 Uiso 1 1 calc R . . C18 C 0.2513(4) 0.5314(3) 0.2791(3) 0.0669(14) Uani 1 1 d . . . H18 H 0.1912 0.5103 0.2400 0.080 Uiso 1 1 calc R . . C19 C 0.2528(4) 0.5300(4) 0.3525(4) 0.0714(15) Uani 1 1 d . . . C20 C 0.3426(4) 0.5629(4) 0.4077(3) 0.0770(16) Uani 1 1 d . . . H20 H 0.3462 0.5642 0.4580 0.092 Uiso 1 1 calc R . . C21 C 0.4278(4) 0.5943(4) 0.3906(3) 0.0702(15) Uani 1 1 d . . . H21 H 0.4876 0.6153 0.4299 0.084 Uiso 1 1 calc R . . C22 C 0.1592(5) 0.4964(5) 0.3724(4) 0.110(2) Uani 1 1 d . . . H22A H 0.1140 0.5474 0.3721 0.165 Uiso 1 1 calc R . . H22B H 0.1847 0.4690 0.4221 0.165 Uiso 1 1 calc R . . H22C H 0.1199 0.4518 0.3355 0.165 Uiso 1 1 calc R . . C23 C 0.7806(4) 0.6805(3) 0.3642(3) 0.0557(12) Uani 1 1 d . . . C24 C 0.8261(4) 0.6206(4) 0.4234(3) 0.0775(17) Uani 1 1 d . . . H24 H 0.7854 0.5734 0.4321 0.093 Uiso 1 1 calc R . . C25 C 0.9295(5) 0.6288(5) 0.4698(4) 0.094(2) Uani 1 1 d . . . H25 H 0.9580 0.5872 0.5094 0.113 Uiso 1 1 calc R . . C26 C 0.9947(4) 0.6992(4) 0.4589(3) 0.0769(16) Uani 1 1 d . . . C27 C 0.9492(4) 0.7568(4) 0.3988(3) 0.0737(15) Uani 1 1 d . . . H27 H 0.9904 0.8024 0.3886 0.088 Uiso 1 1 calc R . . C28 C 0.8449(4) 0.7496(3) 0.3534(3) 0.0619(13) Uani 1 1 d . . . H28 H 0.8162 0.7918 0.3143 0.074 Uiso 1 1 calc R . . C29 C 1.1091(5) 0.7057(5) 0.5104(4) 0.114(3) Uani 1 1 d . . . H29A H 1.1536 0.7006 0.4807 0.171 Uiso 1 1 calc R . . H29B H 1.1253 0.6569 0.5472 0.171 Uiso 1 1 calc R . . H29C H 1.1214 0.7638 0.5363 0.171 Uiso 1 1 calc R . . C30 C 0.6041(4) 0.6423(3) 0.3415(3) 0.0554(12) Uani 1 1 d . . . H30 H 0.629(4) 0.629(3) 0.397(3) 0.071(15) Uiso 1 1 d . . . C31 C 0.5137(4) 0.8221(3) 0.1049(3) 0.0653(14) Uani 1 1 d . . . H31A H 0.5036 0.8881 0.1029 0.078 Uiso 1 1 calc R . . H31B H 0.4670 0.7965 0.0570 0.078 Uiso 1 1 calc R . . C32 C 0.6266(5) 0.8011(3) 0.1146(4) 0.0638(14) Uani 1 1 d . . . C33 C 0.3698(4) 0.7773(4) 0.1458(3) 0.0765(17) Uani 1 1 d . . . H33A H 0.3391 0.8374 0.1341 0.115 Uiso 1 1 calc R . . H33B H 0.3528 0.7514 0.1870 0.115 Uiso 1 1 calc R . . H33C H 0.3419 0.7386 0.1017 0.115 Uiso 1 1 calc R . . C34 C 0.5243(4) 0.8455(3) 0.2350(3) 0.0655(14) Uani 1 1 d . . . H34A H 0.4919 0.9048 0.2217 0.098 Uiso 1 1 calc R . . H34B H 0.5998 0.8514 0.2507 0.098 Uiso 1 1 calc R . . H34C H 0.5065 0.8201 0.2760 0.098 Uiso 1 1 calc R . . C35 C 0.6013(6) 0.6620(5) 0.0417(3) 0.0666(15) Uani 1 1 d . . . C36 C 0.7591(5) 0.6816(5) 0.1479(4) 0.0766(17) Uani 1 1 d . . . H32A H 0.645(4) 0.835(3) 0.067(3) 0.074(14) Uiso 1 1 d . . . H35A H 0.616(3) 0.600(3) 0.046(2) 0.051(13) Uiso 1 1 d . . . H36A H 0.789(5) 0.712(4) 0.194(4) 0.10(2) Uiso 1 1 d . . . H32B H 0.678(4) 0.823(3) 0.162(3) 0.056(13) Uiso 1 1 d . . . H35B H 0.637(5) 0.692(4) 0.009(3) 0.091(18) Uiso 1 1 d . . . H36B H 0.774(4) 0.616(4) 0.147(3) 0.09(2) Uiso 1 1 d . . . H35C H 0.529(6) 0.674(5) 0.020(4) 0.13(3) Uiso 1 1 d . . . H36C H 0.794(5) 0.714(4) 0.112(3) 0.10(2) 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 Mg1 0.0409(9) 0.0374(8) 0.0611(9) -0.0033(7) 0.0187(7) -0.0009(7) N1 0.037(2) 0.040(2) 0.058(2) 0.0002(17) 0.0100(17) -0.0001(18) C1 0.044(3) 0.037(2) 0.061(3) -0.006(2) 0.020(2) 0.001(2) N2 0.041(2) 0.035(2) 0.062(2) 0.0023(17) 0.0126(18) 0.0017(18) C2 0.053(3) 0.053(3) 0.065(3) -0.001(3) 0.021(3) -0.001(3) N3 0.043(2) 0.054(2) 0.062(2) -0.0058(18) 0.0189(19) -0.0085(19) C3 0.057(3) 0.055(3) 0.076(3) -0.011(3) 0.025(3) -0.022(3) N4 0.046(2) 0.057(2) 0.062(2) -0.0038(19) 0.016(2) -0.010(2) C4 0.048(3) 0.056(3) 0.075(3) -0.020(3) 0.023(3) -0.003(3) N5 0.047(2) 0.044(2) 0.067(2) -0.0083(19) 0.0175(19) 0.0020(19) C5 0.050(3) 0.062(3) 0.064(3) -0.003(3) 0.013(2) 0.011(3) N6 0.048(2) 0.041(2) 0.071(2) -0.0046(19) 0.0236(19) 0.0026(19) C6 0.048(3) 0.041(3) 0.068(3) 0.000(2) 0.017(2) -0.001(2) C7 0.050(3) 0.090(4) 0.105(4) -0.028(4) 0.012(3) -0.010(3) C8 0.040(3) 0.040(3) 0.063(3) 0.008(2) 0.020(2) 0.004(2) C9 0.048(3) 0.041(3) 0.075(3) 0.006(3) 0.021(3) 0.007(3) C10 0.069(4) 0.045(3) 0.099(4) 0.015(3) 0.040(3) 0.005(3) C11 0.062(4) 0.062(4) 0.103(4) 0.028(3) 0.040(3) 0.019(3) C12 0.056(4) 0.068(4) 0.101(4) 0.012(3) 0.016(3) 0.014(3) C13 0.054(4) 0.046(3) 0.085(4) -0.002(3) 0.014(3) 0.004(3) C14 0.076(5) 0.086(5) 0.165(7) 0.040(5) 0.042(4) 0.041(4) C15 0.046(3) 0.034(3) 0.058(3) -0.002(2) 0.019(2) 0.000(2) C16 0.048(3) 0.041(3) 0.068(3) -0.001(2) 0.022(2) -0.004(2) C17 0.047(3) 0.060(3) 0.065(3) -0.011(2) 0.019(2) -0.008(3) C18 0.050(3) 0.065(3) 0.087(4) -0.014(3) 0.026(3) -0.010(3) C19 0.066(4) 0.061(3) 0.101(4) -0.005(3) 0.047(3) -0.014(3) C20 0.073(4) 0.087(4) 0.081(4) -0.001(3) 0.040(3) -0.012(3) C21 0.060(3) 0.087(4) 0.066(3) -0.010(3) 0.025(3) -0.015(3) C22 0.085(5) 0.124(6) 0.139(6) 0.007(5) 0.061(4) -0.027(4) C23 0.043(3) 0.059(3) 0.061(3) -0.005(2) 0.014(2) -0.001(2) C24 0.053(4) 0.087(4) 0.083(4) 0.018(3) 0.012(3) -0.017(3) C25 0.056(4) 0.114(5) 0.092(4) 0.022(4) 0.003(3) 0.002(4) C26 0.049(3) 0.086(4) 0.088(4) -0.006(3) 0.016(3) -0.014(3) C27 0.056(4) 0.073(4) 0.090(4) -0.001(3) 0.023(3) -0.016(3) C28 0.050(3) 0.055(3) 0.077(3) -0.004(3) 0.019(3) -0.005(3) C29 0.048(4) 0.146(6) 0.122(5) 0.007(5) -0.002(4) -0.018(4) C30 0.048(3) 0.061(3) 0.055(3) -0.004(2) 0.016(2) -0.006(3) C31 0.079(4) 0.043(3) 0.075(3) 0.004(2) 0.030(3) 0.012(3) C32 0.075(4) 0.042(3) 0.081(4) -0.001(3) 0.036(3) -0.003(3) C33 0.046(3) 0.067(4) 0.105(4) -0.020(3) 0.013(3) 0.008(3) C34 0.072(4) 0.046(3) 0.082(3) -0.018(3) 0.031(3) 0.003(3) C35 0.076(5) 0.058(4) 0.071(3) -0.008(3) 0.033(3) -0.006(4) C36 0.059(4) 0.078(5) 0.095(5) -0.007(4) 0.031(3) -0.001(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 Mg1 N2 2.148(4) . ? Mg1 N3 2.180(4) . ? Mg1 N1 2.222(4) . ? Mg1 N4 2.238(4) . ? Mg1 N5 2.252(4) . ? Mg1 N6 2.293(4) . ? N1 C15 1.319(5) . ? N1 C1 1.408(5) . ? C1 C6 1.378(6) . ? C1 C2 1.386(6) . ? N2 C15 1.302(5) . ? N2 C8 1.383(5) . ? C2 C3 1.377(7) . ? N3 C30 1.308(6) . ? N3 C16 1.406(6) . ? C3 C4 1.380(7) . ? N4 C30 1.329(6) . ? N4 C23 1.406(6) . ? C4 C5 1.377(7) . ? C4 C7 1.498(7) . ? N5 C33 1.463(6) . ? N5 C34 1.480(6) . ? N5 C31 1.485(6) . ? C5 C6 1.375(6) . ? N6 C36 1.463(7) . ? N6 C35 1.469(6) . ? N6 C32 1.481(6) . ? C8 C13 1.365(7) . ? C8 C9 1.396(6) . ? C9 C10 1.376(7) . ? C10 C11 1.371(7) . ? C11 C12 1.373(8) . ? C11 C14 1.516(7) . ? C12 C13 1.381(7) . ? C16 C17 1.367(6) . ? C16 C21 1.407(7) . ? C17 C18 1.389(7) . ? C18 C19 1.375(7) . ? C19 C20 1.369(7) . ? C19 C22 1.523(8) . ? C20 C21 1.380(7) . ? C23 C24 1.375(7) . ? C23 C28 1.391(7) . ? C24 C25 1.362(7) . ? C25 C26 1.413(8) . ? C26 C27 1.363(7) . ? C26 C29 1.505(7) . ? C27 C28 1.365(7) . ? C31 C32 1.501(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 N2 Mg1 N3 99.58(15) . . ? N2 Mg1 N1 61.74(13) . . ? N3 Mg1 N1 99.86(15) . . ? N2 Mg1 N4 99.99(15) . . ? N3 Mg1 N4 61.01(15) . . ? N1 Mg1 N4 152.50(15) . . ? N2 Mg1 N5 160.52(14) . . ? N3 Mg1 N5 93.39(15) . . ? N1 Mg1 N5 101.87(14) . . ? N4 Mg1 N5 98.99(14) . . ? N2 Mg1 N6 91.75(14) . . ? N3 Mg1 N6 162.07(15) . . ? N1 Mg1 N6 97.74(15) . . ? N4 Mg1 N6 103.51(16) . . ? N5 Mg1 N6 79.59(14) . . ? C15 N1 C1 117.1(4) . . ? C15 N1 Mg1 88.2(3) . . ? C1 N1 Mg1 152.9(3) . . ? C6 C1 C2 117.8(4) . . ? C6 C1 N1 119.0(4) . . ? C2 C1 N1 123.2(4) . . ? C15 N2 C8 122.0(4) . . ? C15 N2 Mg1 91.9(3) . . ? C8 N2 Mg1 146.1(3) . . ? C3 C2 C1 121.7(5) . . ? C30 N3 C16 121.4(4) . . ? C30 N3 Mg1 92.5(3) . . ? C16 N3 Mg1 145.8(3) . . ? C2 C3 C4 120.3(5) . . ? C30 N4 C23 117.3(4) . . ? C30 N4 Mg1 89.4(3) . . ? C23 N4 Mg1 149.2(3) . . ? C5 C4 C3 117.9(5) . . ? C5 C4 C7 121.1(5) . . ? C3 C4 C7 121.0(5) . . ? C33 N5 C34 107.7(4) . . ? C33 N5 C31 110.7(4) . . ? C34 N5 C31 109.7(4) . . ? C33 N5 Mg1 110.9(3) . . ? C34 N5 Mg1 110.9(3) . . ? C31 N5 Mg1 107.1(3) . . ? C6 C5 C4 121.9(5) . . ? C36 N6 C35 107.1(5) . . ? C36 N6 C32 110.1(4) . . ? C35 N6 C32 108.9(4) . . ? C36 N6 Mg1 113.1(4) . . ? C35 N6 Mg1 111.7(3) . . ? C32 N6 Mg1 105.9(3) . . ? C5 C6 C1 120.4(4) . . ? C13 C8 N2 117.5(4) . . ? C13 C8 C9 116.3(4) . . ? N2 C8 C9 126.2(4) . . ? C10 C9 C8 122.0(5) . . ? C11 C10 C9 121.0(5) . . ? C10 C11 C12 117.2(5) . . ? C10 C11 C14 121.2(6) . . ? C12 C11 C14 121.6(6) . . ? C11 C12 C13 121.9(5) . . ? C8 C13 C12 121.6(5) . . ? N2 C15 N1 117.8(4) . . ? C17 C16 N3 117.7(4) . . ? C17 C16 C21 115.6(4) . . ? N3 C16 C21 126.7(4) . . ? C16 C17 C18 121.8(5) . . ? C19 C18 C17 122.4(5) . . ? C20 C19 C18 116.5(5) . . ? C20 C19 C22 121.0(6) . . ? C18 C19 C22 122.5(5) . . ? C19 C20 C21 121.7(5) . . ? C20 C21 C16 122.0(5) . . ? C24 C23 C28 117.2(4) . . ? C24 C23 N4 123.3(5) . . ? C28 C23 N4 119.5(4) . . ? C25 C24 C23 121.3(5) . . ? C24 C25 C26 121.4(6) . . ? C27 C26 C25 116.6(5) . . ? C27 C26 C29 123.3(6) . . ? C25 C26 C29 120.1(6) . . ? C26 C27 C28 121.9(5) . . ? C27 C28 C23 121.5(5) . . ? N3 C30 N4 116.5(4) . . ? N5 C31 C32 111.9(4) . . ? N6 C32 C31 110.7(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.315 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.075 #===END data_compound5.CIF _database_code_CSD 185265 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H90 Li2 N12 O7 Zn3' _chemical_formula_weight 1661.73 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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9695(17) _cell_length_b 16.1059(19) _cell_length_c 21.275(3) _cell_angle_alpha 70.803(2) _cell_angle_beta 84.849(2) _cell_angle_gamma 88.306(2) _cell_volume 4824.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8903 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 21046 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.1237 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 23.20 _reflns_number_total 13357 _reflns_number_gt 6072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1999P)^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 13357 _refine_ls_number_parameters 1252 _refine_ls_number_restraints 768 _refine_ls_R_factor_all 0.1944 _refine_ls_R_factor_gt 0.0981 _refine_ls_wR_factor_ref 0.3263 _refine_ls_wR_factor_gt 0.2415 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y ? ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0621(7) 0.0681(8) 0.0709(7) -0.0359(6) -0.0084(6) -0.0010(5) O1 0.064(4) 0.064(4) 0.053(3) -0.025(3) -0.005(3) 0.009(3) N1 0.053(5) 0.061(5) 0.068(5) -0.018(4) -0.006(4) 0.003(4) C1 0.059(5) 0.074(6) 0.067(5) -0.023(5) -0.010(5) -0.001(4) Li1 0.084(13) 0.091(13) 0.071(10) -0.037(9) -0.010(10) 0.009(10) C25B 0.078(18) 0.063(17) 0.078(18) -0.044(11) -0.002(9) 0.006(9) Zn2 0.0713(8) 0.0760(8) 0.0717(8) -0.0399(6) -0.0139(6) 0.0144(6) O2 0.058(4) 0.062(4) 0.070(4) -0.037(3) -0.015(3) 0.004(3) N2 0.072(6) 0.072(6) 0.068(5) -0.039(4) -0.017(4) -0.007(4) C2 0.078(6) 0.064(6) 0.071(5) -0.025(5) -0.005(5) -0.005(5) Li2 0.070(11) 0.083(12) 0.093(12) -0.046(10) -0.014(10) 0.017(9) Zn3 0.0733(8) 0.0670(8) 0.0745(8) -0.0308(6) -0.0007(6) 0.0048(6) O3 0.081(5) 0.064(4) 0.061(4) -0.022(4) -0.001(3) 0.000(3) N3 0.073(5) 0.059(5) 0.070(5) -0.034(4) 0.000(4) 0.002(4) C3 0.085(6) 0.064(6) 0.098(6) -0.037(5) -0.009(6) -0.001(5) O4 0.066(4) 0.077(5) 0.076(4) -0.040(4) -0.013(4) 0.012(3) N4 0.075(6) 0.061(5) 0.072(5) -0.027(4) -0.011(5) 0.000(4) C4 0.073(6) 0.067(6) 0.104(7) -0.015(5) -0.021(6) 0.005(5) O5 0.058(4) 0.084(5) 0.080(4) -0.048(4) -0.005(4) 0.003(4) N5 0.104(7) 0.071(6) 0.067(5) -0.034(5) -0.010(5) -0.011(5) C5 0.086(7) 0.077(6) 0.086(6) -0.015(5) -0.017(6) 0.003(5) O6 0.067(4) 0.080(5) 0.083(4) -0.048(4) -0.012(4) 0.025(4) N6 0.099(7) 0.074(6) 0.080(6) -0.047(5) 0.018(5) -0.017(5) C6 0.090(7) 0.081(6) 0.074(6) -0.023(5) -0.016(5) 0.000(5) O7 0.080(5) 0.096(5) 0.060(4) -0.045(4) -0.021(4) 0.019(4) N7 0.105(7) 0.082(7) 0.078(6) -0.039(5) -0.018(5) 0.017(5) C7 0.125(9) 0.116(8) 0.146(9) -0.031(7) -0.017(7) 0.021(7) N8 0.122(9) 0.108(9) 0.094(8) -0.063(7) -0.025(6) 0.036(7) C8 0.073(6) 0.076(6) 0.068(5) -0.027(5) -0.016(5) -0.008(5) N9 0.109(8) 0.075(6) 0.069(6) -0.017(5) 0.006(5) 0.012(5) C9 0.083(6) 0.081(6) 0.087(6) -0.039(5) -0.009(5) -0.005(5) N10 0.122(8) 0.069(6) 0.070(6) -0.021(5) 0.016(6) 0.007(5) C10 0.114(8) 0.084(7) 0.114(7) -0.046(6) -0.023(6) -0.009(6) N11 0.079(6) 0.073(6) 0.089(6) -0.033(5) -0.001(5) -0.003(5) C11 0.121(8) 0.099(7) 0.116(7) -0.045(6) -0.021(7) -0.014(7) N12 0.080(6) 0.069(6) 0.073(5) -0.029(5) 0.016(5) 0.001(5) C12 0.103(8) 0.103(8) 0.129(8) -0.042(6) -0.037(7) -0.012(6) C13 0.094(7) 0.081(7) 0.102(7) -0.027(6) -0.017(6) -0.018(5) C14 0.167(10) 0.124(9) 0.169(9) -0.083(8) -0.044(8) -0.019(7) C15 0.063(5) 0.063(6) 0.066(5) -0.025(4) -0.013(4) -0.005(5) C16 0.067(6) 0.058(5) 0.057(5) -0.017(4) 0.000(5) -0.006(4) C19 0.081(7) 0.103(7) 0.086(6) -0.034(6) 0.024(6) -0.009(6) C22 0.128(9) 0.137(9) 0.113(8) -0.053(7) 0.028(7) -0.013(7) C23 0.088(7) 0.070(6) 0.077(6) -0.038(5) -0.009(5) -0.014(5) C26 0.131(8) 0.083(7) 0.104(7) -0.047(6) -0.010(6) -0.002(6) C29 0.180(10) 0.141(9) 0.152(9) -0.077(8) -0.027(8) -0.022(7) C30 0.075(6) 0.061(6) 0.067(5) -0.020(5) 0.001(5) -0.005(5) C31 0.084(7) 0.080(6) 0.076(6) -0.036(5) 0.003(5) -0.007(5) C32 0.109(8) 0.104(7) 0.112(7) -0.062(6) 0.008(6) -0.008(6) C33 0.102(8) 0.137(9) 0.133(8) -0.056(7) -0.006(7) -0.009(7) C34 0.116(8) 0.127(8) 0.120(8) -0.064(7) 0.004(7) -0.027(7) C35 0.124(8) 0.101(7) 0.112(7) -0.060(6) 0.002(7) -0.013(7) C36 0.115(8) 0.088(7) 0.092(6) -0.042(6) -0.003(6) -0.016(6) C37 0.152(10) 0.165(10) 0.173(10) -0.080(8) -0.008(8) -0.030(8) C45 0.102(7) 0.096(7) 0.089(6) -0.045(6) 0.008(6) -0.017(6) C46 0.094(7) 0.095(7) 0.073(6) -0.035(5) -0.017(5) 0.013(6) C49 0.109(8) 0.096(7) 0.108(7) -0.014(6) -0.012(7) 0.012(6) C52 0.138(9) 0.115(8) 0.134(8) -0.019(7) -0.018(7) 0.005(7) C53 0.127(8) 0.123(8) 0.088(7) -0.051(6) -0.016(6) 0.027(7) C54 0.135(9) 0.116(8) 0.109(7) -0.061(7) -0.024(7) 0.022(7) C55 0.164(10) 0.129(9) 0.134(8) -0.074(7) -0.021(7) 0.031(7) C56 0.169(10) 0.132(9) 0.131(9) -0.069(7) -0.012(8) 0.025(8) C57 0.190(11) 0.161(10) 0.130(9) -0.076(8) 0.004(8) 0.014(8) C58 0.176(10) 0.141(9) 0.137(9) -0.067(8) 0.012(8) 0.023(8) C59 0.233(12) 0.178(11) 0.181(10) -0.103(9) -0.006(8) 0.028(8) C60 0.104(7) 0.103(8) 0.082(6) -0.034(6) -0.018(6) 0.019(6) C61 0.083(6) 0.083(6) 0.081(6) -0.036(5) 0.002(5) -0.003(5) C64 0.123(8) 0.117(8) 0.092(7) -0.036(6) 0.011(6) -0.007(7) C67 0.184(11) 0.184(11) 0.141(9) -0.066(8) 0.003(8) -0.016(8) C68 0.096(7) 0.065(6) 0.091(7) -0.020(5) 0.007(6) 0.005(5) C69 0.086(8) 0.065(7) 0.064(7) -0.029(6) 0.003(6) -0.012(6) C70 0.099(9) 0.067(8) 0.076(8) -0.026(6) -0.010(7) -0.012(6) C71 0.144(9) 0.114(8) 0.131(8) -0.048(7) 0.000(7) -0.003(7) C74 0.183(11) 0.134(9) 0.168(10) -0.070(8) -0.005(8) -0.007(8) C75 0.111(8) 0.081(7) 0.085(7) -0.030(5) -0.001(6) 0.011(6) C76 0.064(6) 0.081(6) 0.088(6) -0.032(5) -0.005(5) -0.005(5) C77 0.083(7) 0.086(7) 0.101(7) -0.038(6) -0.008(6) -0.001(5) C78 0.101(8) 0.098(7) 0.131(8) -0.047(7) 0.000(7) -0.009(6) C79 0.093(7) 0.132(9) 0.101(7) -0.048(7) -0.005(6) -0.019(7) C80 0.099(8) 0.122(8) 0.119(8) -0.029(7) -0.005(7) 0.005(7) C81 0.086(7) 0.101(7) 0.085(6) -0.026(6) -0.016(6) -0.011(6) C82 0.139(9) 0.167(10) 0.153(9) -0.057(8) -0.023(8) -0.018(8) C83 0.073(6) 0.067(6) 0.088(6) -0.025(5) 0.011(5) 0.004(5) C84 0.126(8) 0.111(8) 0.116(8) -0.066(7) -0.012(7) 0.027(6) C85 0.150(9) 0.125(9) 0.130(8) -0.065(7) -0.011(7) 0.011(7) C86 0.118(8) 0.094(7) 0.112(8) -0.044(6) 0.001(7) 0.016(6) C87 0.117(8) 0.095(7) 0.154(9) -0.048(7) -0.002(7) 0.027(6) C88 0.109(8) 0.101(7) 0.124(8) -0.047(6) -0.007(7) 0.012(6) C89 0.165(10) 0.130(9) 0.156(9) -0.069(8) -0.001(8) 0.013(7) C90 0.061(6) 0.064(6) 0.081(6) -0.018(5) -0.003(5) -0.002(5) C17A 0.074(10) 0.072(10) 0.079(10) -0.025(8) -0.006(8) -0.013(8) C18A 0.063(9) 0.055(9) 0.054(9) -0.013(7) -0.003(7) -0.009(7) C20A 0.072(10) 0.066(9) 0.064(9) -0.028(8) 0.001(8) -0.004(7) C21A 0.061(9) 0.049(9) 0.059(9) -0.022(7) 0.004(7) -0.009(7) C24A 0.097(11) 0.088(10) 0.100(10) -0.048(8) -0.017(8) 0.002(7) C25A 0.152(19) 0.15(2) 0.143(19) -0.064(11) -0.011(9) -0.001(9) C27A 0.127(12) 0.118(11) 0.116(11) -0.046(9) -0.019(9) -0.023(8) C28A 0.112(11) 0.105(10) 0.101(10) -0.055(8) -0.009(8) -0.023(8) C38A 0.073(11) 0.055(10) 0.061(10) -0.023(8) -0.008(8) 0.015(8) C39A 0.078(11) 0.079(11) 0.077(11) -0.027(6) -0.008(5) -0.001(5) C40A 0.086(12) 0.076(11) 0.083(11) -0.030(9) -0.008(9) -0.005(8) C41A 0.092(11) 0.085(11) 0.083(10) -0.037(8) -0.015(8) 0.007(8) C42A 0.114(13) 0.112(12) 0.111(12) -0.057(9) 0.009(9) -0.001(9) C43A 0.082(11) 0.082(10) 0.085(10) -0.044(8) -0.001(8) -0.005(8) C44A 0.115(13) 0.104(12) 0.110(12) -0.047(9) -0.010(9) 0.013(9) C47A 0.046(12) 0.055(12) 0.042(12) -0.010(9) -0.010(9) 0.002(9) C48A 0.070(15) 0.078(15) 0.065(15) -0.014(10) -0.008(10) -0.003(9) C50A 0.045(12) 0.037(11) 0.034(11) -0.009(8) -0.004(8) 0.009(8) C51A 0.023(8) 0.027(8) 0.024(8) -0.008(5) -0.002(5) 0.000(5) C62A 0.082(13) 0.084(12) 0.086(12) -0.032(9) -0.002(9) 0.010(9) C63A 0.088(13) 0.089(12) 0.084(12) -0.025(9) -0.010(9) -0.008(9) C65A 0.111(14) 0.109(14) 0.103(14) -0.036(10) 0.002(9) 0.005(9) C66A 0.092(13) 0.091(12) 0.095(12) -0.037(9) 0.002(9) 0.013(9) C72 0.132(10) 0.076(8) 0.091(8) -0.035(7) -0.004(7) 0.017(7) C73 0.132(10) 0.090(9) 0.091(8) -0.041(7) 0.000(7) 0.019(7) C17B 0.072(10) 0.078(10) 0.073(9) -0.023(7) -0.015(8) -0.003(7) C18B 0.082(10) 0.088(10) 0.096(10) -0.034(8) -0.002(8) -0.002(8) C20B 0.104(11) 0.098(11) 0.095(10) -0.041(8) -0.005(8) -0.003(8) C21B 0.078(10) 0.072(9) 0.077(9) -0.032(7) -0.002(8) 0.006(7) C24B 0.10(2) 0.09(2) 0.11(2) -0.034(11) -0.008(10) -0.002(10) C27B 0.091(17) 0.085(16) 0.096(16) -0.030(10) -0.009(10) -0.002(9) C28B 0.070(14) 0.060(14) 0.070(14) -0.019(9) -0.006(9) -0.003(9) C38B 0.077(11) 0.072(11) 0.077(11) -0.035(8) -0.009(8) 0.014(8) C39B 0.066(11) 0.072(11) 0.062(11) -0.027(8) -0.003(8) 0.000(8) C40B 0.083(11) 0.070(10) 0.076(10) -0.034(8) 0.003(8) -0.001(8) C41B 0.116(12) 0.105(11) 0.101(11) -0.050(9) -0.006(9) 0.008(9) C42B 0.098(11) 0.105(11) 0.096(11) -0.044(9) 0.000(8) 0.002(8) C43B 0.088(10) 0.086(10) 0.079(10) -0.044(8) -0.003(8) -0.009(8) C44B 0.144(14) 0.138(13) 0.132(13) -0.075(10) -0.002(9) 0.005(9) C47B 0.144(13) 0.145(13) 0.125(12) -0.045(9) -0.011(9) -0.007(9) C48B 0.157(14) 0.151(14) 0.130(13) -0.041(9) -0.016(9) -0.015(9) C50B 0.22(2) 0.20(2) 0.20(2) -0.074(11) -0.008(10) 0.007(10) C51B 0.201(17) 0.179(16) 0.176(16) -0.070(10) -0.004(10) 0.014(10) C62B 0.114(12) 0.115(12) 0.101(11) -0.050(9) -0.002(9) -0.017(9) C63B 0.116(13) 0.125(12) 0.107(12) -0.034(9) 0.000(9) -0.005(9) C65B 0.115(12) 0.115(11) 0.098(10) -0.050(9) 0.001(8) -0.004(8) C66B 0.099(11) 0.089(10) 0.080(9) -0.024(8) 0.003(8) 0.009(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.956(6) . ? Zn1 N3 2.040(8) . ? Zn1 N1 2.046(7) . ? Zn1 O5 2.146(6) . ? Zn1 O2 2.162(5) . ? Zn1 Li1 2.774(19) . ? Zn1 Li2 2.819(17) . ? O1 Zn3 1.950(6) . ? O1 Li1 1.991(17) . ? O1 Zn2 1.990(6) . ? O1 Li2 2.029(17) . ? N1 C15 1.294(11) . ? N1 C1 1.452(11) . ? C1 C2 1.384(8) . ? C1 C6 1.394(8) . ? Li1 O4 1.891(19) . ? Li1 O2 1.926(19) . ? Li1 O3 1.92(2) . ? Li1 Zn2 2.796(18) . ? Li1 Zn3 2.820(16) . ? C25B C26 1.389(10) . ? C25B C24B 1.394(10) . ? Zn2 N5 2.003(9) . ? Zn2 N7 2.028(9) . ? Zn2 O7 2.138(6) . ? Zn2 O4 2.166(6) . ? Zn2 Li2 2.840(16) . ? O2 N2 1.379(9) . ? N2 C15 1.346(11) . ? N2 C8 1.399(11) . ? C2 C3 1.380(8) . ? Li2 O6 1.872(19) . ? Li2 O7 1.944(18) . ? Li2 O5 1.93(2) . ? Li2 Zn3 2.817(19) . ? Zn3 N11 2.053(9) . ? Zn3 N9 2.055(9) . ? Zn3 O3 2.147(6) . ? Zn3 O6 2.182(6) . ? O3 N10 1.372(10) . ? N3 C30 1.320(11) . ? N3 C16 1.389(10) . ? C3 C4 1.386(8) . ? O4 N6 1.339(10) . ? N4 C30 1.345(11) . ? N4 O5 1.369(10) . ? N4 C23 1.421(11) . ? C4 C5 1.372(8) . ? C4 C7 1.514(17) . ? N5 C45 1.305(12) . ? N5 C31 1.411(13) . ? C5 C6 1.379(8) . ? O6 N12 1.363(10) . ? N6 C45 1.341(14) . ? N6 C38A 1.45(2) . ? N6 C38B 1.48(2) . ? O7 N8 1.344(12) . ? N7 C60 1.322(13) . ? N7 C46 1.381(13) . ? N8 C60 1.329(15) . ? N8 C53 1.451(14) . ? C8 C9 1.385(8) . ? C8 C13 1.389(9) . ? N9 C75 1.312(13) . ? N9 C61 1.413(12) . ? C9 C10 1.382(8) . ? N10 C75 1.292(13) . ? N10 C68 1.424(13) . ? C10 C11 1.383(9) . ? N11 C90 1.283(12) . ? N11 C76 1.429(13) . ? C11 C12 1.389(9) . ? C11 C14 1.495(16) . ? N12 C90 1.353(12) . ? N12 C83 1.442(12) . ? C12 C13 1.389(9) . ? C16 C17B 1.384(9) . ? C16 C21A 1.389(9) . ? C16 C21B 1.392(9) . ? C16 C17A 1.408(10) . ? C19 C18A 1.387(9) . ? C19 C18B 1.386(10) . ? C19 C20A 1.394(10) . ? C19 C20B 1.397(10) . ? C19 C22 1.503(15) . ? C23 C28B 1.383(10) . ? C23 C24A 1.386(9) . ? C23 C28A 1.392(10) . ? C23 C24B 1.392(10) . ? C26 C27B 1.383(10) . ? C26 C27A 1.388(10) . ? C26 C25A 1.392(10) . ? C26 C29 1.546(17) . ? C31 C32 1.384(9) . ? C31 C36 1.387(9) . ? C32 C33 1.401(9) . ? C33 C34 1.373(9) . ? C34 C35 1.384(9) . ? C34 C37 1.487(19) . ? C35 C36 1.381(9) . ? C46 C47B 1.379(10) . ? C46 C47A 1.385(10) . ? C46 C51B 1.385(10) . ? C46 C51A 1.392(10) . ? C49 C48B 1.376(10) . ? C49 C50B 1.389(10) . ? C49 C50A 1.398(10) . ? C49 C48A 1.398(10) . ? C49 C52 1.518(17) . ? C53 C54 1.382(9) . ? C53 C58 1.386(9) . ? C54 C55 1.392(9) . ? C55 C56 1.377(9) . ? C56 C57 1.365(9) . ? C56 C59 1.506(19) . ? C57 C58 1.389(9) . ? C61 C66A 1.388(10) . ? C61 C62B 1.391(10) . ? C61 C62A 1.401(10) . ? C61 C66B 1.404(9) . ? C64 C63B 1.381(10) . ? C64 C65A 1.385(10) . ? C64 C65B 1.387(10) . ? C64 C63A 1.388(10) . ? C64 C67 1.607(18) . ? C68 C69 1.375(9) . ? C68 C73 1.390(9) . ? C69 C70 1.365(9) . ? C70 C71 1.380(9) . ? C71 C72 1.393(9) . ? C71 C74 1.547(18) . ? C76 C77 1.348(14) . ? C76 C81 1.399(16) . ? C77 C78 1.400(17) . ? C78 C79 1.303(18) . ? C79 C80 1.355(18) . ? C79 C82 1.582(19) . ? C80 C81 1.400(17) . ? C83 C84 1.347(16) . ? C83 C88 1.363(16) . ? C84 C85 1.386(16) . ? C85 C86 1.335(18) . ? C86 C87 1.349(18) . ? C86 C89 1.486(17) . ? C87 C88 1.379(17) . ? C17A C18A 1.392(10) . ? C20A C21A 1.390(10) . ? C24A C25A 1.400(10) . ? C27A C28A 1.394(10) . ? C38A C43A 1.389(10) . ? C38A C39A 1.390(10) . ? C39A C40A 1.389(10) . ? C40A C41A 1.383(10) . ? C41A C42A 1.393(10) . ? C41A C44A 1.54(3) . ? C42A C43A 1.393(10) . ? C47A C48A 1.392(10) . ? C50A C51A 1.398(10) . ? C62A C63A 1.386(10) . ? C65A C66A 1.390(10) . ? C72 C73 1.387(9) . ? C17B C18B 1.391(10) . ? C20B C21B 1.392(10) . ? C27B C28B 1.390(10) . ? C38B C43B 1.380(10) . ? C38B C39B 1.387(10) . ? C39B C40B 1.394(10) . ? C40B C41B 1.388(10) . ? C41B C42B 1.379(10) . ? C41B C44B 1.51(3) . ? C42B C43B 1.380(10) . ? C47B C48B 1.383(10) . ? C50B C51B 1.397(10) . ? C62B C63B 1.384(10) . ? C65B C66B 1.393(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N3 122.7(3) . . ? O1 Zn1 N1 118.5(3) . . ? N3 Zn1 N1 118.7(3) . . ? O1 Zn1 O5 89.0(2) . . ? N3 Zn1 O5 78.9(3) . . ? N1 Zn1 O5 104.4(3) . . ? O1 Zn1 O2 89.5(2) . . ? N3 Zn1 O2 100.5(2) . . ? N1 Zn1 O2 77.7(3) . . ? O5 Zn1 O2 177.8(2) . . ? O1 Zn1 Li1 45.8(4) . . ? N3 Zn1 Li1 117.9(4) . . ? N1 Zn1 Li1 102.4(4) . . ? O5 Zn1 Li1 134.6(4) . . ? O2 Zn1 Li1 43.8(4) . . ? O1 Zn1 Li2 46.0(4) . . ? N3 Zn1 Li2 105.6(4) . . ? N1 Zn1 Li2 117.6(4) . . ? O5 Zn1 Li2 43.1(4) . . ? O2 Zn1 Li2 135.5(4) . . ? Li1 Zn1 Li2 91.9(5) . . ? Zn3 O1 Zn1 121.0(3) . . ? Zn3 O1 Li1 91.4(6) . . ? Zn1 O1 Li1 89.3(6) . . ? Zn3 O1 Zn2 118.6(3) . . ? Zn1 O1 Zn2 120.4(3) . . ? Li1 O1 Zn2 89.2(6) . . ? Zn3 O1 Li2 90.1(6) . . ? Zn1 O1 Li2 90.0(6) . . ? Li1 O1 Li2 178.5(8) . . ? Zn2 O1 Li2 89.9(5) . . ? C15 N1 C1 115.4(8) . . ? C15 N1 Zn1 115.1(6) . . ? C1 N1 Zn1 129.5(6) . . ? C2 C1 C6 117.9(9) . . ? C2 C1 N1 119.3(8) . . ? C6 C1 N1 122.7(8) . . ? O4 Li1 O2 119.0(10) . . ? O4 Li1 O3 120.5(10) . . ? O2 Li1 O3 118.3(10) . . ? O4 Li1 O1 95.9(8) . . ? O2 Li1 O1 95.6(8) . . ? O3 Li1 O1 93.2(7) . . ? O4 Li1 Zn1 112.4(9) . . ? O2 Li1 Zn1 50.9(5) . . ? O3 Li1 Zn1 114.9(8) . . ? O1 Li1 Zn1 44.8(4) . . ? O4 Li1 Zn2 50.7(4) . . ? O2 Li1 Zn2 118.0(9) . . ? O3 Li1 Zn2 111.1(7) . . ? O1 Li1 Zn2 45.4(4) . . ? Zn1 Li1 Zn2 75.9(5) . . ? O4 Li1 Zn3 116.7(7) . . ? O2 Li1 Zn3 112.5(8) . . ? O3 Li1 Zn3 49.5(4) . . ? O1 Li1 Zn3 43.7(4) . . ? Zn1 Li1 Zn3 74.8(4) . . ? Zn2 Li1 Zn3 74.2(4) . . ? C26 C25B C24B 111(3) . . ? O1 Zn2 N5 123.9(3) . . ? O1 Zn2 N7 118.6(3) . . ? N5 Zn2 N7 117.4(4) . . ? O1 Zn2 O7 88.6(2) . . ? N5 Zn2 O7 103.1(3) . . ? N7 Zn2 O7 80.1(3) . . ? O1 Zn2 O4 87.8(2) . . ? N5 Zn2 O4 78.3(3) . . ? N7 Zn2 O4 102.3(3) . . ? O7 Zn2 O4 176.3(2) . . ? O1 Zn2 Li1 45.4(4) . . ? N5 Zn2 Li1 105.7(4) . . ? N7 Zn2 Li1 115.7(5) . . ? O7 Zn2 Li1 133.9(4) . . ? O4 Zn2 Li1 42.5(4) . . ? O1 Zn2 Li2 45.6(4) . . ? N5 Zn2 Li2 120.0(5) . . ? N7 Zn2 Li2 104.5(4) . . ? O7 Zn2 Li2 43.2(4) . . ? O4 Zn2 Li2 133.1(4) . . ? Li1 Zn2 Li2 91.0(5) . . ? N2 O2 Li1 111.9(8) . . ? N2 O2 Zn1 107.6(4) . . ? Li1 O2 Zn1 85.3(5) . . ? C15 N2 O2 118.9(7) . . ? C15 N2 C8 124.8(8) . . ? O2 N2 C8 116.1(7) . . ? C3 C2 C1 121.0(9) . . ? O6 Li2 O7 117.1(10) . . ? O6 Li2 O5 121.1(9) . . ? O7 Li2 O5 120.6(10) . . ? O6 Li2 O1 94.4(8) . . ? O7 Li2 O1 93.1(7) . . ? O5 Li2 O1 93.3(7) . . ? O6 Li2 Zn3 50.7(5) . . ? O7 Li2 Zn3 108.6(8) . . ? O5 Li2 Zn3 116.1(8) . . ? O1 Li2 Zn3 43.8(4) . . ? O6 Li2 Zn1 111.9(8) . . ? O7 Li2 Zn1 116.0(7) . . ? O5 Li2 Zn1 49.5(4) . . ? O1 Li2 Zn1 43.9(4) . . ? Zn3 Li2 Zn1 74.2(4) . . ? O6 Li2 Zn2 115.3(8) . . ? O7 Li2 Zn2 48.8(4) . . ? O5 Li2 Zn2 110.5(7) . . ? O1 Li2 Zn2 44.5(3) . . ? Zn3 Li2 Zn2 73.6(4) . . ? Zn1 Li2 Zn2 74.5(4) . . ? O1 Zn3 N11 120.8(3) . . ? O1 Zn3 N9 124.7(3) . . ? N11 Zn3 N9 114.4(4) . . ? O1 Zn3 O3 87.9(2) . . ? N11 Zn3 O3 103.8(3) . . ? N9 Zn3 O3 78.3(3) . . ? O1 Zn3 O6 87.6(2) . . ? N11 Zn3 O6 77.5(3) . . ? N9 Zn3 O6 105.5(3) . . ? O3 Zn3 O6 175.3(3) . . ? O1 Zn3 Li1 44.9(4) . . ? N11 Zn3 Li1 120.0(4) . . ? N9 Zn3 Li1 105.1(5) . . ? O3 Zn3 Li1 43.0(4) . . ? O6 Zn3 Li1 132.4(4) . . ? O1 Zn3 Li2 46.1(4) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 23.20 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.966 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.102 #===END data_compound6.CIF _database_code_CSD 185266 _audit_creation_method WinGX routine CIF_UPDATE _chemical_name_systematic ; [(eta4-O)(di(p-tolyl)formamidinato)6 Zinc(II)] ; _chemical_name_common '[(eta4-O)Zn(FTolP)6]' _chemical_melting_point ? _chemical_formula_moiety 'C90 H90 N12 O Zn4' _chemical_formula_sum ? _chemical_formula_weight 1617.22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-y+1/4, -z+1/4, x' 'z, -x+1/4, -y+1/4' '-y+1/4, z, -x+1/4' '-z+1/4, -x+1/4, y' '-z+1/4, x, -y+1/4' 'y, -z+1/4, -x+1/4' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' 'z, x+1/2, y+1/2' 'y, z+1/2, x+1/2' '-y+1/4, -z+3/4, x+1/2' 'z, -x+3/4, -y+3/4' '-y+1/4, z+1/2, -x+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+1/4, x+1/2, -y+3/4' 'y, -z+3/4, -x+3/4' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' 'z+1/2, x, y+1/2' 'y+1/2, z, x+1/2' '-y+3/4, -z+1/4, x+1/2' 'z+1/2, -x+1/4, -y+3/4' '-y+3/4, z, -x+3/4' '-z+3/4, -x+1/4, y+1/2' '-z+3/4, x, -y+3/4' 'y+1/2, -z+1/4, -x+3/4' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' 'z+1/2, x+1/2, y' 'y+1/2, z+1/2, x' '-y+3/4, -z+3/4, x' 'z+1/2, -x+3/4, -y+1/4' '-y+3/4, z+1/2, -x+1/4' '-z+3/4, -x+3/4, y' '-z+3/4, x+1/2, -y+1/4' 'y+1/2, -z+3/4, -x+1/4' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' 'y-1/4, z-1/4, -x' '-z, x-1/4, y-1/4' 'y-1/4, -z, x-1/4' 'z-1/4, x-1/4, -y' 'z-1/4, -x, y-1/4' '-y, z-1/4, x-1/4' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' '-z, -x+1/2, -y+1/2' '-y, -z+1/2, -x+1/2' 'y-1/4, z+1/4, -x+1/2' '-z, x+1/4, y+1/4' 'y-1/4, -z+1/2, x+1/4' 'z-1/4, x+1/4, -y+1/2' 'z-1/4, -x+1/2, y+1/4' '-y, z+1/4, x+1/4' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' '-z+1/2, -x, -y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/4, z-1/4, -x+1/2' '-z+1/2, x-1/4, y+1/4' 'y+1/4, -z, x+1/4' 'z+1/4, x-1/4, -y+1/2' 'z+1/4, -x, y+1/4' '-y+1/2, z-1/4, x+1/4' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' '-z+1/2, -x+1/2, -y' '-y+1/2, -z+1/2, -x' 'y+1/4, z+1/4, -x' '-z+1/2, x+1/4, y-1/4' 'y+1/4, -z+1/2, x-1/4' 'z+1/4, x+1/4, -y' 'z+1/4, -x+1/2, y-1/4' '-y+1/2, z+1/4, x-1/4' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fd-3 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 0 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _cell_length_a 28.594(3) _cell_length_b 28.594(3) _cell_length_c 28.594(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 23380(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6736 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26319 _diffrn_reflns_av_R_equivalents 0.2819 _diffrn_reflns_av_sigmaI/netI 0.1263 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 23.28 _reflns_number_total 1409 _reflns_number_gt 633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^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 SHELXL _refine_ls_extinction_coef 0.00035(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1409 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1848 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.66383(3) 0.16383(3) 0.08617(3) 0.0546(7) Uani 1 3 d S . . O1 O 0.625 0.125 0.125 0.047(4) Uani 1 12 d SP . . N1 N 0.7259(2) 0.1304(2) 0.0842(2) 0.0558(17) Uani 1 1 d . . . C1 C 0.7526(3) 0.1212(3) 0.0437(3) 0.068(2) Uani 1 1 d . . . C2 C 0.7463(3) 0.1486(3) 0.0036(3) 0.068(2) Uani 1 1 d . . . H2 H 0.7248 0.1729 0.0038 0.082 Uiso 1 1 calc R . . C3 C 0.7717(4) 0.1397(4) -0.0360(4) 0.098(3) Uani 1 1 d . . . H3 H 0.7675 0.1587 -0.0621 0.117 Uiso 1 1 calc R . . C4 C 0.8034(5) 0.1030(5) -0.0383(5) 0.132(5) Uani 1 1 d . . . C5 C 0.8090(5) 0.0762(5) 0.0008(5) 0.145(6) Uani 1 1 d . . . H5 H 0.8308 0.0521 0 0.174 Uiso 1 1 calc R . . C6 C 0.7836(4) 0.0834(4) 0.0418(4) 0.105(4) Uani 1 1 d . . . H6 H 0.7872 0.0636 0.0673 0.126 Uiso 1 1 calc R . . C7 C 0.8328(7) 0.0938(6) -0.0825(6) 0.239(10) Uani 1 1 d . . . H7A H 0.864 0.0852 -0.0736 0.359 Uiso 1 1 calc R . . H7B H 0.8337 0.1216 -0.1013 0.359 Uiso 1 1 calc R . . H7C H 0.8189 0.0688 -0.1001 0.359 Uiso 1 1 calc R . . C8 C 0.7482(4) 0.125 0.125 0.059(3) Uani 1 2 d S . . H8 H 0.7807 0.125 0.125 0.07 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0546(7) 0.0546(7) 0.0546(7) 0.0014(5) 0.0014(5) -0.0014(5) O1 0.047(4) 0.047(4) 0.047(4) 0 0 0 N1 0.056(4) 0.062(4) 0.050(4) -0.005(3) 0.007(4) 0.002(3) C1 0.057(6) 0.078(7) 0.068(7) -0.001(5) 0.010(5) 0.002(5) C2 0.064(6) 0.081(7) 0.060(6) 0.005(5) 0.013(5) -0.014(5) C3 0.103(9) 0.111(9) 0.080(8) 0.015(6) 0.030(7) -0.010(7) C4 0.152(12) 0.140(12) 0.103(10) 0.014(9) 0.071(9) 0.032(10) C5 0.153(12) 0.148(13) 0.135(12) 0.021(10) 0.078(10) 0.069(10) C6 0.123(9) 0.101(8) 0.090(8) 0.024(6) 0.038(7) 0.039(7) C7 0.30(2) 0.26(2) 0.156(15) 0.043(13) 0.168(16) 0.123(17) C8 0.042(7) 0.064(8) 0.071(9) 0.002(6) 0 0 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9231(15) . ? Zn1 N1 2.015(6) . ? Zn1 N1 2.015(6) 44_545 ? Zn1 N1 2.015(6) 33 ? O1 Zn1 1.9231(15) 10_655 ? O1 Zn1 1.9231(15) 12_655 ? O1 Zn1 1.9231(15) 11 ? N1 C8 1.338(8) . ? N1 C1 1.413(9) . ? C1 C6 1.398(12) . ? C1 C2 1.400(11) . ? C2 C3 1.369(12) . ? C3 C4 1.387(15) . ? C4 C5 1.365(15) . ? C4 C7 1.539(14) . ? C5 C6 1.395(13) . ? C8 N1 1.338(8) 11 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N1 104.52(18) . . ? O1 Zn1 N1 104.52(18) . 44_545 ? N1 Zn1 N1 113.93(15) . 44_545 ? O1 Zn1 N1 104.52(18) . 33 ? N1 Zn1 N1 113.93(15) . 33 ? N1 Zn1 N1 113.93(15) 44_545 33 ? Zn1 O1 Zn1 109.5 10_655 . ? Zn1 O1 Zn1 109.5 10_655 12_655 ? Zn1 O1 Zn1 109.5 . 12_655 ? Zn1 O1 Zn1 109.5 10_655 11 ? Zn1 O1 Zn1 109.5 . 11 ? Zn1 O1 Zn1 109.5 12_655 11 ? C8 N1 C1 115.7(7) . . ? C8 N1 Zn1 116.8(6) . . ? C1 N1 Zn1 126.0(6) . . ? C6 C1 C2 118.7(8) . . ? C6 C1 N1 121.3(8) . . ? C2 C1 N1 119.8(8) . . ? C3 C2 C1 120.4(9) . . ? C2 C3 C4 121.7(10) . . ? C5 C4 C3 117.6(11) . . ? C5 C4 C7 120.7(13) . . ? C3 C4 C7 121.7(13) . . ? C4 C5 C6 123.0(11) . . ? C5 C6 C1 118.5(10) . . ? N1 C8 N1 123.1(10) . 11 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.797 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.078