# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_address ; State Key Laboratory of Structural chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian, 350002, China ; _publ_contact_author_email yyg@fjirsm.ac.cn _publ_contact_author_fax 86-591-83714946 _publ_contact_author_phone 86-591-83711523 loop_ _publ_author_name 'Yuan-Gen Yao' 'Xin Zhang' #============================================================================= data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 873031' #TrackingRef '- Compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Mg N2 O14 Zn2' _chemical_formula_sum 'C32 H30 Mg N2 O14 Zn2' _chemical_formula_weight 821.67 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' Zn Zn 0.2839 1.4301 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.3223(18) _cell_length_b 10.6962(7) _cell_length_c 15.7966(12) _cell_angle_alpha 90.00 _cell_angle_beta 111.051(9) _cell_angle_gamma 90.00 _cell_volume 3677.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1990 _cell_measurement_theta_min 2.6908 _cell_measurement_theta_max 29.1522 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6577 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3238 _reflns_number_gt 2589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3238 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 Zn1 Zn -0.092348(18) 1.34522(3) -0.93765(3) 0.02823(19) Uani 1 1 d . . . Mg1 Mg -0.2500 1.2500 -1.0000 0.0140(3) Uani 1 2 d S . . C1 C -0.13652(17) 1.1130(4) -0.7615(2) 0.0359(9) Uani 1 1 d . . . C2 C -0.08667(19) 1.0361(4) -0.7197(3) 0.0505(11) Uani 1 1 d . . . H2A H -0.0513 1.0453 -0.7334 0.061 Uiso 1 1 calc R . . C3 C -0.0883(2) 0.9462(4) -0.6584(3) 0.0515(11) Uani 1 1 d . . . H3A H -0.0543 0.8953 -0.6313 0.062 Uiso 1 1 calc R . . C4 C -0.14055(17) 0.9312(3) -0.6369(3) 0.0361(9) Uani 1 1 d . . . C5 C -0.18968(17) 1.0097(4) -0.6776(3) 0.0416(10) Uani 1 1 d . . . H5A H -0.2246 1.0029 -0.6624 0.050 Uiso 1 1 calc R . . C6 C -0.18816(17) 1.0979(4) -0.7403(3) 0.0405(10) Uani 1 1 d . . . H6A H -0.2225 1.1476 -0.7684 0.049 Uiso 1 1 calc R . . C7 C -0.13488(18) 1.2085(3) -0.8292(2) 0.0351(9) Uani 1 1 d . . . C8 C -0.14419(18) 0.8360(3) -0.5704(3) 0.0364(9) Uani 1 1 d . . . C9 C -0.22253(18) 1.6346(3) -0.9955(3) 0.0341(9) Uani 1 1 d . . . C10 C -0.18895(19) 1.7362(4) -0.9490(3) 0.0458(10) Uani 1 1 d . . . H10A H -0.1474 1.7270 -0.9148 0.055 Uiso 1 1 calc R . . C11 C -0.21657(19) 1.8502(3) -0.9530(3) 0.0436(10) Uani 1 1 d . . . H11A H -0.1939 1.9174 -0.9206 0.052 Uiso 1 1 calc R . . C12 C -0.19287(17) 1.5091(3) -0.9919(2) 0.0307(8) Uani 1 1 d . . . C13 C 0.0420(2) 1.4000(4) -0.8951(3) 0.0475(11) Uani 1 1 d . . . C14 C 0.0521(2) 1.2991(5) -0.9525(4) 0.0672(14) Uani 1 1 d . . . H14A H 0.0134 1.2627 -0.9885 0.101 Uiso 1 1 calc R . . H14B H 0.0781 1.2359 -0.9145 0.101 Uiso 1 1 calc R . . H14C H 0.0715 1.3332 -0.9917 0.101 Uiso 1 1 calc R . . C15 C 0.1525(2) 1.4423(6) -0.8275(4) 0.0804(18) Uani 1 1 d . . . H15A H 0.1549 1.3757 -0.8669 0.121 Uiso 1 1 calc R . . H15B H 0.1750 1.4193 -0.7656 0.121 Uiso 1 1 calc R . . H15C H 0.1699 1.5169 -0.8421 0.121 Uiso 1 1 calc R . . C16 C 0.0771(3) 1.5637(6) -0.7861(4) 0.095(2) Uani 1 1 d . . . H16A H 0.0337 1.5713 -0.7997 0.142 Uiso 1 1 calc R . . H16B H 0.0928 1.6408 -0.8000 0.142 Uiso 1 1 calc R . . H16C H 0.0973 1.5450 -0.7229 0.142 Uiso 1 1 calc R . . O1 O -0.08421(12) 1.2293(2) -0.83819(19) 0.0453(7) Uani 1 1 d . . . O2 O -0.18330(12) 1.2647(2) -0.87241(17) 0.0389(6) Uani 1 1 d . . . O3 O -0.10076(13) 0.7571(2) -0.54298(18) 0.0422(7) Uani 1 1 d . . . O4 O -0.18900(13) 0.8384(2) -0.5460(2) 0.0423(7) Uani 1 1 d . . . O5 O -0.13572(12) 1.5028(2) -0.94835(19) 0.0380(6) Uani 1 1 d . . . O6 O -0.22525(11) 1.4209(2) -1.03283(17) 0.0336(6) Uani 1 1 d . . . O7 O -0.01156(12) 1.4269(3) -0.9000(2) 0.0513(8) Uani 1 1 d . . . N1 N 0.08849(17) 1.4648(4) -0.8394(3) 0.0620(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0342(3) 0.0217(3) 0.0317(3) 0.00051(15) 0.0153(2) 0.00077(16) Mg1 0.0178(7) 0.0088(6) 0.0166(7) -0.0003(5) 0.0077(6) 0.0008(5) C1 0.038(2) 0.0363(19) 0.031(2) 0.0082(17) 0.0101(16) -0.0010(17) C2 0.042(2) 0.060(3) 0.063(3) 0.030(2) 0.034(2) 0.010(2) C3 0.045(2) 0.055(3) 0.064(3) 0.033(2) 0.031(2) 0.018(2) C4 0.036(2) 0.038(2) 0.039(2) 0.0091(17) 0.0205(18) 0.0009(17) C5 0.031(2) 0.047(2) 0.052(2) 0.0137(19) 0.0213(18) -0.0028(18) C6 0.031(2) 0.043(2) 0.043(2) 0.0148(18) 0.0079(17) 0.0051(17) C7 0.048(2) 0.0295(19) 0.0241(18) 0.0040(15) 0.0086(17) -0.0036(18) C8 0.041(2) 0.032(2) 0.040(2) 0.0030(16) 0.0189(19) -0.0018(17) C9 0.041(2) 0.0197(17) 0.045(2) -0.0008(15) 0.0202(18) -0.0009(15) C10 0.036(2) 0.032(2) 0.064(3) -0.0045(19) 0.011(2) 0.0019(17) C11 0.042(2) 0.024(2) 0.058(3) -0.0065(17) 0.011(2) -0.0017(16) C12 0.039(2) 0.0206(17) 0.038(2) 0.0028(15) 0.0197(17) 0.0039(16) C13 0.045(3) 0.051(3) 0.045(2) 0.013(2) 0.014(2) -0.011(2) C14 0.060(3) 0.070(3) 0.078(4) 0.006(3) 0.031(3) 0.004(3) C15 0.034(3) 0.124(5) 0.070(3) 0.035(3) 0.003(2) -0.021(3) C16 0.091(4) 0.121(5) 0.071(4) -0.029(4) 0.028(3) -0.057(4) O1 0.0423(16) 0.0449(16) 0.0497(17) 0.0195(13) 0.0176(14) -0.0015(13) O2 0.0453(16) 0.0348(14) 0.0302(14) 0.0045(11) 0.0059(12) -0.0008(12) O3 0.0504(17) 0.0403(15) 0.0441(16) 0.0136(13) 0.0267(14) 0.0067(13) O4 0.0468(16) 0.0356(15) 0.0565(18) 0.0105(12) 0.0330(15) -0.0008(12) O5 0.0389(15) 0.0223(12) 0.0529(17) -0.0008(11) 0.0167(13) 0.0014(11) O6 0.0407(14) 0.0201(12) 0.0396(14) 0.0006(11) 0.0138(12) -0.0015(11) O7 0.0345(16) 0.0498(17) 0.070(2) -0.0032(15) 0.0198(14) -0.0098(13) N1 0.048(2) 0.091(3) 0.042(2) 0.009(2) 0.0098(17) -0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.941(2) . ? Zn1 O3 1.941(3) 6_575 ? Zn1 O1 1.956(3) . ? Zn1 O7 1.965(3) . ? Mg1 O6 2.039(2) 7_473 ? Mg1 O6 2.039(2) . ? Mg1 O4 2.047(2) 4_453 ? Mg1 O4 2.047(2) 6_575 ? Mg1 O2 2.063(2) . ? Mg1 O2 2.063(2) 7_473 ? C1 C6 1.371(5) . ? C1 C2 1.383(5) . ? C1 C7 1.489(5) . ? C2 C3 1.375(6) . ? C2 H2A 0.9300 . ? C3 C4 1.387(5) . ? C3 H3A 0.9300 . ? C4 C5 1.379(5) . ? C4 C8 1.488(5) . ? C5 C6 1.377(5) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O2 1.244(4) . ? C7 O1 1.260(5) . ? C8 O4 1.237(5) . ? C8 O3 1.270(4) . ? C9 C11 1.370(6) 7_483 ? C9 C10 1.387(5) . ? C9 C12 1.501(5) . ? C10 C11 1.369(5) . ? C10 H10A 0.9300 . ? C11 C9 1.370(5) 7_483 ? C11 H11A 0.9300 . ? C12 O6 1.237(4) . ? C12 O5 1.263(4) . ? C13 O7 1.257(5) . ? C13 N1 1.321(5) . ? C13 C14 1.483(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N1 1.456(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N1 1.435(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? O3 Zn1 1.941(3) 6_576 ? O4 Mg1 2.047(2) 4_443 ? 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 O5 Zn1 O3 121.70(12) . 6_575 ? O5 Zn1 O1 121.15(12) . . ? O3 Zn1 O1 106.38(13) 6_575 . ? O5 Zn1 O7 93.06(11) . . ? O3 Zn1 O7 107.51(12) 6_575 . ? O1 Zn1 O7 103.44(12) . . ? O6 Mg1 O6 180.0 7_473 . ? O6 Mg1 O4 91.57(10) 7_473 4_453 ? O6 Mg1 O4 88.43(10) . 4_453 ? O6 Mg1 O4 88.43(10) 7_473 6_575 ? O6 Mg1 O4 91.57(10) . 6_575 ? O4 Mg1 O4 180.000(1) 4_453 6_575 ? O6 Mg1 O2 90.15(10) 7_473 . ? O6 Mg1 O2 89.85(10) . . ? O4 Mg1 O2 89.68(11) 4_453 . ? O4 Mg1 O2 90.32(11) 6_575 . ? O6 Mg1 O2 89.85(10) 7_473 7_473 ? O6 Mg1 O2 90.15(10) . 7_473 ? O4 Mg1 O2 90.32(11) 4_453 7_473 ? O4 Mg1 O2 89.68(11) 6_575 7_473 ? O2 Mg1 O2 180.0(2) . 7_473 ? C6 C1 C2 118.3(3) . . ? C6 C1 C7 120.5(3) . . ? C2 C1 C7 121.1(3) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 118.1(3) . . ? C5 C4 C8 119.8(3) . . ? C3 C4 C8 122.0(3) . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C1 C6 C5 120.6(3) . . ? C1 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? O2 C7 O1 123.8(3) . . ? O2 C7 C1 118.2(3) . . ? O1 C7 C1 118.0(3) . . ? O4 C8 O3 124.6(3) . . ? O4 C8 C4 118.4(3) . . ? O3 C8 C4 117.1(3) . . ? C11 C9 C10 119.3(3) 7_483 . ? C11 C9 C12 119.6(3) 7_483 . ? C10 C9 C12 121.1(3) . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C9 120.3(4) . 7_483 ? C10 C11 H11A 119.9 . . ? C9 C11 H11A 119.9 7_483 . ? O6 C12 O5 124.8(3) . . ? O6 C12 C9 118.4(3) . . ? O5 C12 C9 116.8(3) . . ? O7 C13 N1 118.8(4) . . ? O7 C13 C14 120.2(4) . . ? N1 C13 C14 121.1(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C7 O1 Zn1 112.2(2) . . ? C7 O2 Mg1 135.8(2) . . ? C8 O3 Zn1 119.3(2) . 6_576 ? C8 O4 Mg1 150.9(2) . 4_443 ? C12 O5 Zn1 120.6(2) . . ? C12 O6 Mg1 136.6(2) . . ? C13 O7 Zn1 137.8(3) . . ? C13 N1 C16 119.8(4) . . ? C13 N1 C15 123.9(5) . . ? C16 N1 C15 116.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.838 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.083 #=========================END data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 873032' #TrackingRef '- Compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Ca N2 O10 Zn' _chemical_formula_sum 'C24 H26 Ca N2 O10 Zn' _chemical_formula_weight 607.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 10.3110(4) _cell_length_b 18.4014(13) _cell_length_c 14.3666(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.825(5) _cell_angle_gamma 90.00 _cell_volume 2685.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2332 _cell_measurement_theta_min 2.5108 _cell_measurement_theta_max 29.2244 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84483 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10032 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4705 _reflns_number_gt 3378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+2.5251P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4705 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Zn1 Zn 0.29259(4) 0.81383(3) -1.05302(3) 0.02439(16) Uani 1 1 d . . . Ca1 Ca 0.37633(8) 0.69185(5) -0.82110(6) 0.0278(2) Uani 1 1 d . . . C1 C 0.3244(4) 0.5920(2) -1.1207(3) 0.0289(10) Uani 1 1 d . . . C2 C 0.3693(4) 0.5275(3) -1.0780(3) 0.0379(11) Uani 1 1 d . . . H2A H 0.3967 0.5260 -1.0129 0.045 Uiso 1 1 calc R . . C3 C 0.3741(4) 0.4650(3) -1.1307(3) 0.0386(11) Uani 1 1 d . . . H3A H 0.4083 0.4225 -1.1012 0.046 Uiso 1 1 calc R . . C4 C 0.3285(4) 0.4652(2) -1.2266(3) 0.0249(9) Uani 1 1 d . . . C5 C 0.2784(5) 0.5291(3) -1.2686(3) 0.0395(12) Uani 1 1 d . . . H5A H 0.2441 0.5297 -1.3328 0.047 Uiso 1 1 calc R . . C6 C 0.2786(5) 0.5923(3) -1.2164(3) 0.0413(12) Uani 1 1 d . . . H6A H 0.2476 0.6353 -1.2462 0.050 Uiso 1 1 calc R . . C7 C 0.3291(4) 0.6598(2) -1.0630(3) 0.0314(10) Uani 1 1 d . . . C8 C 0.3323(4) 0.3968(2) -1.2832(3) 0.0302(10) Uani 1 1 d . . . C9 C -0.0418(4) 0.7921(2) -0.9301(3) 0.0303(10) Uani 1 1 d . . . C10 C -0.1037(4) 0.7519(3) -0.8695(3) 0.0366(11) Uani 1 1 d . . . H10A H -0.0549 0.7196 -0.8276 0.044 Uiso 1 1 calc R . . C11 C -0.2372(4) 0.7590(3) -0.8703(3) 0.0333(11) Uani 1 1 d . . . H11A H -0.2774 0.7320 -0.8284 0.040 Uiso 1 1 calc R . . C12 C -0.3111(4) 0.8060(2) -0.9330(3) 0.0254(9) Uani 1 1 d . . . C13 C -0.2482(4) 0.8465(3) -0.9938(3) 0.0367(11) Uani 1 1 d . . . H13A H -0.2970 0.8782 -1.0365 0.044 Uiso 1 1 calc R . . C14 C -0.1144(4) 0.8404(3) -0.9917(3) 0.0406(12) Uani 1 1 d . . . H14A H -0.0732 0.8687 -1.0316 0.049 Uiso 1 1 calc R . . C15 C 0.1041(4) 0.7834(3) -0.9310(3) 0.0343(11) Uani 1 1 d . . . C16 C -0.4572(4) 0.8108(2) -0.9371(3) 0.0273(10) Uani 1 1 d . . . C17 C 0.2916(9) 0.8076(4) -0.6523(4) 0.086(2) Uani 1 1 d . . . C18 C 0.1354(6) 0.8048(4) -0.6504(5) 0.092(3) Uani 1 1 d . . . H18A H 0.1116 0.8449 -0.6140 0.138 Uiso 1 1 calc R . . H18B H 0.1142 0.7600 -0.6222 0.138 Uiso 1 1 calc R . . H18C H 0.0876 0.8078 -0.7137 0.138 Uiso 1 1 calc R . . C19 C 0.2943(9) 0.9148(5) -0.5552(6) 0.137(4) Uani 1 1 d . . . H19A H 0.2011 0.9086 -0.5594 0.206 Uiso 1 1 calc R . . H19B H 0.3119 0.9616 -0.5799 0.206 Uiso 1 1 calc R . . H19C H 0.3362 0.9115 -0.4903 0.206 Uiso 1 1 calc R . . C20 C 0.4960(7) 0.8567(5) -0.6129(6) 0.131(4) Uani 1 1 d . . . H20A H 0.5159 0.8164 -0.6504 0.197 Uiso 1 1 calc R . . H20B H 0.5441 0.8519 -0.5499 0.197 Uiso 1 1 calc R . . H20C H 0.5207 0.9012 -0.6402 0.197 Uiso 1 1 calc R . . C21 C 0.2518(10) 0.5386(5) -0.7193(6) 0.122(4) Uani 1 1 d D . . C22 C 0.3720(6) 0.4843(4) -0.6635(6) 0.103(3) Uani 1 1 d D . . H22A H 0.3350 0.4496 -0.6255 0.154 Uiso 1 1 calc R . . H22B H 0.4367 0.5131 -0.6240 0.154 Uiso 1 1 calc R . . H22C H 0.4127 0.4590 -0.7095 0.154 Uiso 1 1 calc R . . C23 C 0.0468(6) 0.5772(4) -0.7513(6) 0.102(3) Uani 1 1 d . . . H23A H 0.0849 0.6114 -0.7892 0.152 Uiso 1 1 calc R . . H23B H 0.0065 0.6028 -0.7055 0.152 Uiso 1 1 calc R . . H23C H -0.0186 0.5488 -0.7911 0.152 Uiso 1 1 calc R . . C24 C 0.1178(8) 0.4679(4) -0.6357(6) 0.110(3) Uani 1 1 d . . . H24A H 0.1887 0.4378 -0.6055 0.164 Uiso 1 1 calc R . . H24B H 0.0528 0.4383 -0.6739 0.164 Uiso 1 1 calc R . . H24C H 0.0785 0.4925 -0.5885 0.164 Uiso 1 1 calc R . . O1 O 0.2902(3) 0.71702(17) -1.1076(2) 0.0409(8) Uani 1 1 d . . . O2 O 0.3727(3) 0.65643(18) -0.9772(2) 0.0435(8) Uani 1 1 d . . . O3 O 0.2419(3) 0.39192(17) -1.3543(2) 0.0419(8) Uani 1 1 d . . . O4 O 0.4181(3) 0.35070(17) -1.2571(2) 0.0368(8) Uani 1 1 d . . . O5 O 0.1538(3) 0.82868(18) -0.9807(2) 0.0428(8) Uani 1 1 d . . . O6 O 0.1633(3) 0.7327(2) -0.8852(2) 0.0544(10) Uani 1 1 d . . . O7 O -0.5227(3) 0.83865(18) -1.0115(2) 0.0368(8) Uani 1 1 d . . . O8 O -0.5064(3) 0.78667(17) -0.8704(2) 0.0347(7) Uani 1 1 d . . . O9 O 0.3361(4) 0.7593(3) -0.6965(3) 0.0740(13) Uani 1 1 d . . . O10 O 0.2891(4) 0.5855(2) -0.7709(3) 0.0682(12) Uani 1 1 d . . . N1 N 0.3459(9) 0.8579(4) -0.6102(5) 0.115(3) Uani 1 1 d . . . N2 N 0.1677(11) 0.5206(4) -0.6943(5) 0.156(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0170(2) 0.0242(3) 0.0315(3) 0.0020(2) 0.00273(18) 0.0012(2) Ca1 0.0220(4) 0.0311(5) 0.0310(5) 0.0033(4) 0.0062(3) 0.0031(4) C1 0.029(2) 0.025(2) 0.032(2) -0.003(2) 0.0033(18) -0.0019(19) C2 0.042(3) 0.038(3) 0.029(2) 0.000(2) -0.007(2) 0.007(2) C3 0.043(3) 0.031(3) 0.038(3) 0.002(2) -0.004(2) 0.011(2) C4 0.022(2) 0.025(2) 0.026(2) -0.0015(19) -0.0015(17) -0.0014(18) C5 0.050(3) 0.038(3) 0.025(2) -0.003(2) -0.008(2) 0.002(2) C6 0.065(3) 0.023(3) 0.034(3) 0.003(2) 0.001(2) 0.006(2) C7 0.025(2) 0.031(3) 0.037(3) -0.006(2) 0.0021(19) 0.002(2) C8 0.024(2) 0.032(3) 0.034(2) -0.001(2) 0.0043(19) -0.003(2) C9 0.0156(19) 0.042(3) 0.033(2) -0.001(2) 0.0038(17) 0.0029(19) C10 0.021(2) 0.048(3) 0.040(3) 0.013(2) 0.0029(19) 0.007(2) C11 0.023(2) 0.041(3) 0.036(3) 0.009(2) 0.0059(19) 0.004(2) C12 0.0172(19) 0.030(2) 0.028(2) -0.0023(19) 0.0024(16) 0.0017(18) C13 0.020(2) 0.051(3) 0.039(3) 0.018(2) 0.0028(18) 0.005(2) C14 0.027(2) 0.054(3) 0.042(3) 0.015(2) 0.009(2) -0.001(2) C15 0.018(2) 0.043(3) 0.041(3) -0.009(2) 0.005(2) 0.004(2) C16 0.0191(19) 0.025(2) 0.038(2) -0.005(2) 0.0044(19) -0.0018(18) C17 0.147(8) 0.070(5) 0.034(4) 0.014(4) -0.006(4) 0.003(5) C18 0.062(4) 0.138(8) 0.084(5) 0.022(5) 0.030(4) 0.026(4) C19 0.178(10) 0.100(7) 0.138(8) -0.047(6) 0.040(7) 0.038(7) C20 0.047(4) 0.186(10) 0.160(8) 0.041(8) 0.016(5) -0.002(5) C21 0.174(10) 0.096(7) 0.118(7) -0.040(6) 0.087(7) -0.086(7) C22 0.061(4) 0.086(6) 0.161(8) 0.045(5) 0.018(5) 0.022(4) C23 0.064(4) 0.093(6) 0.142(7) 0.046(5) -0.001(4) 0.022(4) C24 0.110(6) 0.097(6) 0.129(7) 0.047(5) 0.042(5) -0.040(5) O1 0.052(2) 0.0251(18) 0.0437(19) -0.0017(15) 0.0036(15) 0.0044(16) O2 0.052(2) 0.042(2) 0.0333(19) -0.0098(16) -0.0023(15) 0.0115(17) O3 0.0351(17) 0.0366(19) 0.0466(19) -0.0159(16) -0.0136(15) 0.0074(15) O4 0.0315(16) 0.0306(18) 0.0452(19) -0.0027(15) -0.0020(14) 0.0079(14) O5 0.0216(15) 0.046(2) 0.065(2) -0.0021(17) 0.0200(15) 0.0016(15) O6 0.0238(17) 0.078(3) 0.061(2) 0.021(2) 0.0071(15) 0.0154(18) O7 0.0168(14) 0.047(2) 0.0442(18) 0.0145(16) -0.0006(13) 0.0042(14) O8 0.0209(14) 0.043(2) 0.0417(18) 0.0059(15) 0.0096(13) -0.0047(14) O9 0.092(3) 0.083(3) 0.054(2) -0.012(2) 0.033(2) 0.029(3) O10 0.064(2) 0.056(3) 0.090(3) 0.028(2) 0.027(2) -0.009(2) N1 0.168(8) 0.093(6) 0.084(5) 0.001(4) 0.023(5) 0.020(5) N2 0.263(11) 0.117(7) 0.116(6) -0.037(5) 0.111(7) -0.125(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 O5 1.926(3) . ? Zn1 O1 1.945(3) . ? Zn1 O3 1.951(3) 2_552 ? Zn1 O7 1.951(3) 1_655 ? Ca1 O9 2.274(4) . ? Ca1 O8 2.302(3) 1_655 ? Ca1 O10 2.319(4) . ? Ca1 O2 2.330(3) . ? Ca1 O6 2.355(3) . ? Ca1 O4 2.357(3) 3_663 ? C1 C6 1.376(6) . ? C1 C2 1.379(6) . ? C1 C7 1.494(6) . ? C2 C3 1.382(6) . ? C2 H2A 0.9300 . ? C3 C4 1.378(6) . ? C3 H3A 0.9300 . ? C4 C5 1.381(6) . ? C4 C8 1.503(6) . ? C5 C6 1.383(6) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O2 1.239(5) . ? C7 O1 1.262(5) . ? C8 O4 1.237(5) . ? C8 O3 1.263(5) . ? C9 C14 1.380(6) . ? C9 C10 1.381(6) . ? C9 C15 1.515(5) . ? C10 C11 1.381(5) . ? C10 H10A 0.9300 . ? C11 C12 1.381(6) . ? C11 H11A 0.9300 . ? C12 C13 1.390(6) . ? C12 C16 1.500(5) . ? C13 C14 1.379(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O6 1.240(5) . ? C15 O5 1.261(6) . ? C16 O8 1.240(5) . ? C16 O7 1.271(5) . ? C17 N1 1.192(9) . ? C17 O9 1.225(8) . ? C17 C18 1.617(10) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N1 1.466(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N1 1.555(10) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N2 1.047(9) . ? C21 O10 1.241(9) . ? C21 C22 1.685(11) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N2 1.721(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N2 1.436(9) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O3 Zn1 1.951(3) 2_542 ? O4 Ca1 2.357(3) 3_663 ? O7 Zn1 1.951(3) 1_455 ? O8 Ca1 2.302(3) 1_455 ? 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 O5 Zn1 O1 112.83(14) . . ? O5 Zn1 O3 101.44(14) . 2_552 ? O1 Zn1 O3 114.28(14) . 2_552 ? O5 Zn1 O7 125.35(14) . 1_655 ? O1 Zn1 O7 106.39(14) . 1_655 ? O3 Zn1 O7 95.22(12) 2_552 1_655 ? O9 Ca1 O8 90.26(14) . 1_655 ? O9 Ca1 O10 94.78(16) . . ? O8 Ca1 O10 170.73(13) 1_655 . ? O9 Ca1 O2 159.30(14) . . ? O8 Ca1 O2 80.72(12) 1_655 . ? O10 Ca1 O2 96.89(14) . . ? O9 Ca1 O6 81.41(14) . . ? O8 Ca1 O6 98.15(12) 1_655 . ? O10 Ca1 O6 90.31(14) . . ? O2 Ca1 O6 81.50(12) . . ? O9 Ca1 O4 94.36(13) . 3_663 ? O8 Ca1 O4 85.51(11) 1_655 3_663 ? O10 Ca1 O4 86.36(13) . 3_663 ? O2 Ca1 O4 103.37(11) . 3_663 ? O6 Ca1 O4 174.38(12) . 3_663 ? C6 C1 C2 118.7(4) . . ? C6 C1 C7 121.6(4) . . ? C2 C1 C7 119.7(4) . . ? C1 C2 C3 120.8(4) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 C8 120.2(4) . . ? C5 C4 C8 121.3(4) . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 120.5(4) . . ? C1 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? O2 C7 O1 125.2(4) . . ? O2 C7 C1 118.8(4) . . ? O1 C7 C1 116.0(4) . . ? O4 C8 O3 126.0(4) . . ? O4 C8 C4 119.6(4) . . ? O3 C8 C4 114.4(4) . . ? C14 C9 C10 119.4(4) . . ? C14 C9 C15 119.6(4) . . ? C10 C9 C15 121.0(4) . . ? C9 C10 C11 120.8(4) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C10 120.2(4) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 118.8(4) . . ? C11 C12 C16 120.1(4) . . ? C13 C12 C16 121.1(4) . . ? C14 C13 C12 120.9(4) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C9 119.9(4) . . ? C13 C14 H14A 120.1 . . ? C9 C14 H14A 120.1 . . ? O6 C15 O5 125.9(4) . . ? O6 C15 C9 118.3(4) . . ? O5 C15 C9 115.7(4) . . ? O8 C16 O7 124.4(4) . . ? O8 C16 C12 119.3(4) . . ? O7 C16 C12 116.3(4) . . ? N1 C17 O9 129.9(10) . . ? N1 C17 C18 113.5(8) . . ? O9 C17 C18 116.6(7) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 O10 141.6(13) . . ? N2 C21 C22 103.6(10) . . ? O10 C21 C22 114.8(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 O1 Zn1 125.4(3) . . ? C7 O2 Ca1 152.5(3) . . ? C8 O3 Zn1 128.9(3) . 2_542 ? C8 O4 Ca1 155.6(3) . 3_663 ? C15 O5 Zn1 128.5(3) . . ? C15 O6 Ca1 142.1(3) . . ? C16 O7 Zn1 120.9(3) . 1_455 ? C16 O8 Ca1 144.5(3) . 1_455 ? C17 O9 Ca1 159.7(4) . . ? C21 O10 Ca1 161.5(5) . . ? C17 N1 C19 130.3(10) . . ? C17 N1 C20 111.1(8) . . ? C19 N1 C20 118.5(8) . . ? C21 N2 C24 144.6(14) . . ? C21 N2 C23 102.8(9) . . ? C24 N2 C23 112.6(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.812 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.080 #=========================END data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 873033' #TrackingRef '- Compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 N2 O10 Sr Zn' _chemical_formula_sum 'C24 H26 N2 O10 Sr Zn' _chemical_formula_weight 655.48 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 10.4064(5) _cell_length_b 18.5332(9) _cell_length_c 14.4984(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.153(5) _cell_angle_gamma 90.00 _cell_volume 2752.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3349 _cell_measurement_theta_min 2.4845 _cell_measurement_theta_max 29.1573 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53572 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10340 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4843 _reflns_number_gt 3815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4843 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 Sr1 Sr 1.10654(3) 0.69530(2) 0.31751(3) 0.02743(16) Uani 1 1 d . . . Zn1 Zn 1.19417(4) 0.81875(2) 0.55600(3) 0.02167(16) Uani 1 1 d . . . C1 C 1.3167(4) 0.9716(2) 0.7708(3) 0.0258(9) Uani 1 1 d . . . C2 C 1.3766(5) 0.9729(2) 0.8631(3) 0.0410(12) Uani 1 1 d . . . H2A H 1.4161 0.9313 0.8907 0.049 Uiso 1 1 calc R . . C3 C 1.3787(4) 1.0353(2) 0.9151(3) 0.0418(12) Uani 1 1 d . . . H3A H 1.4154 1.0346 0.9784 0.050 Uiso 1 1 calc R . . C4 C 1.3271(4) 1.0984(2) 0.8744(3) 0.0251(9) Uani 1 1 d . . . C5 C 1.2668(5) 1.0974(2) 0.7818(3) 0.0399(11) Uani 1 1 d . . . H5A H 1.2298 1.1393 0.7534 0.048 Uiso 1 1 calc R . . C6 C 1.2613(4) 1.0338(2) 0.7313(3) 0.0368(11) Uani 1 1 d . . . H6A H 1.2191 1.0333 0.6692 0.044 Uiso 1 1 calc R . . C7 C 1.3126(4) 0.9027(2) 0.7145(3) 0.0280(9) Uani 1 1 d . . . C8 C 1.3377(4) 1.1669(2) 0.9313(3) 0.0277(9) Uani 1 1 d . . . C9 C 0.7967(4) 0.8105(2) 0.4389(3) 0.0267(10) Uani 1 1 d . . . C10 C 0.7222(4) 0.7643(2) 0.3760(3) 0.0338(10) Uani 1 1 d . . . H10A H 0.7609 0.7381 0.3335 0.041 Uiso 1 1 calc R . . C11 C 0.5892(4) 0.7572(3) 0.3765(3) 0.0379(11) Uani 1 1 d . . . H11A H 0.5401 0.7251 0.3353 0.046 Uiso 1 1 calc R . . C12 C 0.5293(4) 0.7968(2) 0.4369(3) 0.0316(10) Uani 1 1 d . . . C13 C 0.6026(4) 0.8432(3) 0.4983(3) 0.0380(11) Uani 1 1 d . . . H13A H 0.5628 0.8706 0.5390 0.046 Uiso 1 1 calc R . . C14 C 0.7372(4) 0.8498(3) 0.5000(3) 0.0366(11) Uani 1 1 d . . . H14A H 0.7864 0.8808 0.5427 0.044 Uiso 1 1 calc R . . C15 C 0.9414(4) 0.8158(2) 0.4409(3) 0.0258(9) Uani 1 1 d . . . C16 C 0.3852(4) 0.7877(3) 0.4373(3) 0.0384(11) Uani 1 1 d . . . C17 C 1.2384(11) 0.5348(5) 0.2179(6) 0.130(4) Uani 1 1 d D . . C18 C 1.1246(6) 0.4795(4) 0.1641(6) 0.099(3) Uani 1 1 d D . . H18A H 1.1636 0.4449 0.1281 0.149 Uiso 1 1 calc R . . H18B H 1.0596 0.5067 0.1232 0.149 Uiso 1 1 calc R . . H18C H 1.0844 0.4547 0.2098 0.149 Uiso 1 1 calc R . . C19 C 1.4440(6) 0.5765(4) 0.2517(6) 0.099(3) Uani 1 1 d . . . H19A H 1.4048 0.6103 0.2886 0.149 Uiso 1 1 calc R . . H19B H 1.4828 0.6021 0.2060 0.149 Uiso 1 1 calc R . . H19C H 1.5100 0.5494 0.2918 0.149 Uiso 1 1 calc R . . C20 C 1.3794(7) 0.4666(4) 0.1392(6) 0.111(3) Uani 1 1 d . . . H20A H 1.3092 0.4362 0.1099 0.167 Uiso 1 1 calc R . . H20B H 1.4444 0.4376 0.1775 0.167 Uiso 1 1 calc R . . H20C H 1.4176 0.4905 0.0919 0.167 Uiso 1 1 calc R . . C21 C 1.2047(9) 0.8147(4) 0.1443(5) 0.082(2) Uani 1 1 d . . . C22 C 1.3571(7) 0.8079(4) 0.1481(6) 0.098(3) Uani 1 1 d . . . H22A H 1.3857 0.8447 0.1098 0.146 Uiso 1 1 calc R . . H22B H 1.3768 0.7613 0.1252 0.146 Uiso 1 1 calc R . . H22C H 1.4014 0.8135 0.2116 0.146 Uiso 1 1 calc R . . C23 C 1.0053(7) 0.8686(6) 0.0939(7) 0.133(4) Uani 1 1 d . . . H23A H 0.9773 0.8309 0.1313 0.200 Uiso 1 1 calc R . . H23B H 0.9617 0.8634 0.0301 0.200 Uiso 1 1 calc R . . H23C H 0.9842 0.9147 0.1175 0.200 Uiso 1 1 calc R . . C24 C 1.2109(11) 0.9166(5) 0.0420(7) 0.155(4) Uani 1 1 d . . . H24A H 1.3026 0.9063 0.0500 0.232 Uiso 1 1 calc R . . H24B H 1.1985 0.9646 0.0635 0.232 Uiso 1 1 calc R . . H24C H 1.1727 0.9126 -0.0231 0.232 Uiso 1 1 calc R . . O1 O 1.3924(3) 0.85425(16) 0.7419(2) 0.0389(8) Uani 1 1 d . . . O2 O 1.2242(3) 0.89956(16) 0.6434(2) 0.0404(8) Uani 1 1 d . . . O3 O 1.2946(3) 1.22341(15) 0.8874(2) 0.0383(8) Uani 1 1 d . . . O4 O 1.3902(3) 1.16426(17) 1.0153(2) 0.0438(8) Uani 1 1 d . . . O5 O 1.0091(2) 0.84043(17) 0.5156(2) 0.0359(8) Uani 1 1 d . . . O6 O 0.9870(3) 0.79585(16) 0.3711(2) 0.0327(7) Uani 1 1 d . . . O7 O 0.3353(3) 0.83251(18) 0.4872(2) 0.0437(8) Uani 1 1 d . . . O8 O 0.3260(3) 0.7401(2) 0.3899(3) 0.0649(12) Uani 1 1 d . . . O9 O 1.2021(4) 0.5829(2) 0.2678(3) 0.0763(13) Uani 1 1 d . . . O10 O 1.1489(5) 0.7711(3) 0.1899(3) 0.0834(14) Uani 1 1 d . . . N1 N 1.3294(9) 0.5201(4) 0.1973(5) 0.134(4) Uani 1 1 d . . . N2 N 1.1465(7) 0.8636(4) 0.0979(5) 0.110(2) Uani 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 Sr1 0.0249(3) 0.0288(3) 0.0287(3) -0.00601(17) 0.00519(19) -0.00445(15) Zn1 0.0182(3) 0.0188(3) 0.0271(3) -0.00205(19) 0.0015(2) -0.00172(17) C1 0.025(2) 0.021(2) 0.029(2) -0.0013(18) -0.0029(18) -0.0012(16) C2 0.060(3) 0.024(2) 0.033(3) -0.001(2) -0.009(2) 0.019(2) C3 0.051(3) 0.034(3) 0.033(3) -0.006(2) -0.014(2) 0.015(2) C4 0.029(2) 0.022(2) 0.024(2) -0.0013(17) 0.0028(17) 0.0007(17) C5 0.064(3) 0.019(2) 0.032(3) 0.003(2) -0.006(2) 0.007(2) C6 0.055(3) 0.026(2) 0.021(2) -0.0045(19) -0.015(2) 0.006(2) C7 0.023(2) 0.023(2) 0.038(3) -0.0045(19) 0.0037(19) -0.0031(17) C8 0.031(2) 0.025(2) 0.027(2) -0.0020(19) 0.0050(19) 0.0002(18) C9 0.018(2) 0.031(2) 0.030(2) -0.0015(18) 0.0011(18) -0.0021(16) C10 0.026(2) 0.041(3) 0.033(3) -0.009(2) 0.0033(19) 0.0002(19) C11 0.025(2) 0.049(3) 0.040(3) -0.015(2) 0.006(2) -0.012(2) C12 0.019(2) 0.042(3) 0.034(3) 0.005(2) 0.0044(19) -0.0022(18) C13 0.024(2) 0.052(3) 0.039(3) -0.014(2) 0.008(2) 0.005(2) C14 0.026(2) 0.047(3) 0.037(3) -0.018(2) 0.003(2) -0.003(2) C15 0.019(2) 0.023(2) 0.035(3) 0.0028(19) 0.0041(19) 0.0014(16) C16 0.022(2) 0.050(3) 0.043(3) 0.007(2) 0.002(2) -0.001(2) C17 0.204(11) 0.103(7) 0.105(7) 0.043(6) 0.092(8) 0.103(8) C18 0.075(4) 0.068(5) 0.150(8) -0.044(5) 0.007(5) -0.018(4) C19 0.067(4) 0.093(6) 0.135(7) -0.044(6) 0.011(5) -0.022(4) C20 0.104(6) 0.099(6) 0.138(7) -0.062(6) 0.041(5) 0.032(5) C21 0.126(7) 0.068(5) 0.048(4) -0.012(4) 0.002(4) -0.006(5) C22 0.076(5) 0.126(8) 0.096(6) -0.020(5) 0.031(5) -0.017(4) C23 0.051(4) 0.190(11) 0.155(9) -0.021(8) 0.007(5) 0.004(5) C24 0.214(11) 0.115(8) 0.144(9) 0.062(7) 0.054(8) -0.051(8) O1 0.0417(17) 0.0246(16) 0.045(2) -0.0046(15) -0.0068(15) 0.0116(14) O2 0.0398(17) 0.0297(17) 0.0424(19) -0.0157(15) -0.0178(15) 0.0074(14) O3 0.0527(19) 0.0204(16) 0.0388(19) -0.0035(14) -0.0005(15) 0.0043(14) O4 0.062(2) 0.0339(18) 0.0307(19) -0.0095(15) -0.0054(16) 0.0069(16) O5 0.0158(13) 0.0467(19) 0.0424(19) -0.0157(16) -0.0023(13) -0.0004(13) O6 0.0257(15) 0.0352(17) 0.0394(19) -0.0017(14) 0.0114(14) 0.0020(12) O7 0.0237(15) 0.044(2) 0.068(2) 0.0060(18) 0.0211(16) 0.0017(14) O8 0.0278(17) 0.093(3) 0.073(3) -0.030(3) 0.0085(18) -0.023(2) O9 0.077(3) 0.059(3) 0.100(4) -0.030(3) 0.036(3) 0.007(2) O10 0.105(3) 0.092(3) 0.060(3) 0.016(3) 0.034(3) -0.034(3) N1 0.210(9) 0.107(6) 0.107(6) 0.036(5) 0.085(6) 0.109(6) N2 0.124(6) 0.101(6) 0.106(6) -0.001(5) 0.024(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O10 2.425(4) . ? Sr1 O6 2.442(3) . ? Sr1 O9 2.469(4) . ? Sr1 O1 2.480(3) 4_575 ? Sr1 O8 2.482(3) 1_655 ? Sr1 O4 2.486(3) 2_746 ? Zn1 O7 1.933(3) 1_655 ? Zn1 O3 1.943(3) 2_746 ? Zn1 O2 1.951(3) . ? Zn1 O5 1.954(3) . ? C1 C6 1.368(6) . ? C1 C2 1.373(6) . ? C1 C7 1.512(5) . ? C2 C3 1.378(6) . ? C2 H2A 0.9300 . ? C3 C4 1.376(6) . ? C3 H3A 0.9300 . ? C4 C5 1.379(6) . ? C4 C8 1.507(5) . ? C5 C6 1.384(6) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O1 1.240(5) . ? C7 O2 1.256(5) . ? C8 O4 1.245(5) . ? C8 O3 1.265(5) . ? C9 C14 1.376(6) . ? C9 C10 1.384(6) . ? C9 C15 1.505(5) . ? C10 C11 1.391(5) . ? C10 H10A 0.9300 . ? C11 C12 1.374(6) . ? C11 H11A 0.9300 . ? C12 C13 1.369(6) . ? C12 C16 1.510(6) . ? C13 C14 1.401(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O6 1.247(5) . ? C15 O5 1.269(5) . ? C16 O8 1.218(6) . ? C16 O7 1.270(6) . ? C17 N1 1.078(9) . ? C17 O9 1.248(8) . ? C17 C18 1.655(11) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N1 1.675(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N1 1.456(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N2 1.222(9) . ? C21 O10 1.251(8) . ? C21 C22 1.582(11) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N2 1.464(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N2 1.504(9) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O1 Sr1 2.480(3) 4_676 ? O3 Zn1 1.943(3) 2_756 ? O4 Sr1 2.486(3) 2_756 ? O7 Zn1 1.933(3) 1_455 ? O8 Sr1 2.482(3) 1_455 ? 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 O10 Sr1 O6 88.41(14) . . ? O10 Sr1 O9 97.41(16) . . ? O6 Sr1 O9 172.00(11) . . ? O10 Sr1 O1 98.46(13) . 4_575 ? O6 Sr1 O1 87.42(10) . 4_575 ? O9 Sr1 O1 86.31(12) . 4_575 ? O10 Sr1 O8 81.47(15) . 1_655 ? O6 Sr1 O8 95.31(11) . 1_655 ? O9 Sr1 O8 90.99(14) . 1_655 ? O1 Sr1 O8 177.27(11) 4_575 1_655 ? O10 Sr1 O4 154.87(14) . 2_746 ? O6 Sr1 O4 77.66(11) . 2_746 ? O9 Sr1 O4 98.77(13) . 2_746 ? O1 Sr1 O4 101.65(10) 4_575 2_746 ? O8 Sr1 O4 79.15(12) 1_655 2_746 ? O7 Zn1 O3 110.07(13) 1_655 2_746 ? O7 Zn1 O2 100.64(14) 1_655 . ? O3 Zn1 O2 115.68(13) 2_746 . ? O7 Zn1 O5 128.09(14) 1_655 . ? O3 Zn1 O5 107.25(13) 2_746 . ? O2 Zn1 O5 94.22(12) . . ? C6 C1 C2 118.7(4) . . ? C6 C1 C7 121.0(4) . . ? C2 C1 C7 120.3(4) . . ? C1 C2 C3 120.5(4) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 C8 119.8(4) . . ? C5 C4 C8 121.4(4) . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C1 C6 C5 121.3(4) . . ? C1 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? O1 C7 O2 125.5(4) . . ? O1 C7 C1 119.0(4) . . ? O2 C7 C1 115.5(4) . . ? O4 C8 O3 125.5(4) . . ? O4 C8 C4 118.6(4) . . ? O3 C8 C4 115.9(4) . . ? C14 C9 C10 119.2(4) . . ? C14 C9 C15 121.0(4) . . ? C10 C9 C15 119.7(4) . . ? C9 C10 C11 119.9(4) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 121.0(4) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 119.1(4) . . ? C13 C12 C16 120.5(4) . . ? C11 C12 C16 120.4(4) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C9 C14 C13 120.3(4) . . ? C9 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? O6 C15 O5 124.5(4) . . ? O6 C15 C9 119.2(4) . . ? O5 C15 C9 116.3(4) . . ? O8 C16 O7 125.3(4) . . ? O8 C16 C12 118.8(4) . . ? O7 C16 C12 115.8(4) . . ? N1 C17 O9 135.5(12) . . ? N1 C17 C18 107.6(9) . . ? O9 C17 C18 116.9(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 O10 122.6(9) . . ? N2 C21 C22 118.3(8) . . ? O10 C21 C22 119.1(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 O1 Sr1 155.3(3) . 4_676 ? C7 O2 Zn1 125.4(3) . . ? C8 O3 Zn1 123.4(3) . 2_756 ? C8 O4 Sr1 150.8(3) . 2_756 ? C15 O5 Zn1 123.5(3) . . ? C15 O6 Sr1 140.6(3) . . ? C16 O7 Zn1 129.2(3) . 1_455 ? C16 O8 Sr1 144.8(3) . 1_455 ? C17 O9 Sr1 161.8(5) . . ? C21 O10 Sr1 160.4(5) . . ? C17 N1 C20 139.0(11) . . ? C17 N1 C19 107.4(9) . . ? C20 N1 C19 113.6(7) . . ? C21 N2 C23 117.7(9) . . ? C21 N2 C24 123.7(9) . . ? C23 N2 C24 118.5(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.982 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.086 #=========================END data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 873034' #TrackingRef '- Compounds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H16 Ba N2 O16 Zn2' _chemical_formula_sum 'C30 H16 Ba N2 O16 Zn2' _chemical_formula_weight 928.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.1637(6) _cell_length_b 19.0644(6) _cell_length_c 12.6634(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.767(5) _cell_angle_gamma 90.00 _cell_volume 3375.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2764 _cell_measurement_theta_min 2.7509 _cell_measurement_theta_max 29.1091 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 2.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.673 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5895 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2929 _reflns_number_gt 2565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+11.1675P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00266(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2929 _refine_ls_number_parameters 263 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _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 Zn1 Zn -0.37959(3) 0.79359(2) -0.96173(4) 0.01897(13) Uani 1 1 d . . . Ba1 Ba -0.5000 0.680283(15) -1.2500 0.01896(12) Uani 1 2 d S . . C1 C -0.3528(3) 0.65212(19) -0.9334(3) 0.0224(8) Uani 1 1 d . . . C2 C -0.3169(3) 0.58588(18) -0.8675(3) 0.0213(8) Uani 1 1 d . . . C3 C -0.3655(3) 0.5237(2) -0.9118(3) 0.0302(9) Uani 1 1 d . . . H3A H -0.4151 0.5236 -0.9837 0.036 Uiso 1 1 calc R . . C4 C -0.3406(3) 0.4623(2) -0.8495(4) 0.0340(10) Uani 1 1 d . . . H4A H -0.3740 0.4212 -0.8793 0.041 Uiso 1 1 calc R . . C5 C -0.2661(3) 0.46136(19) -0.7428(3) 0.0248(8) Uani 1 1 d . . . C6 C -0.2152(3) 0.5222(2) -0.7010(3) 0.0292(9) Uani 1 1 d . . . H6A H -0.1633 0.5214 -0.6310 0.035 Uiso 1 1 calc R . . C7 C -0.2404(3) 0.58451(19) -0.7623(3) 0.0275(9) Uani 1 1 d . . . H7A H -0.2061 0.6253 -0.7327 0.033 Uiso 1 1 calc R . . C8 C -0.2449(3) 0.39452(19) -0.6739(3) 0.0244(8) Uani 1 1 d . . . C9 C -0.5738(3) 0.77343(19) -1.0329(4) 0.0262(9) Uani 1 1 d . . . C10 C -0.6656(3) 0.7617(2) -1.0154(3) 0.0249(8) Uani 1 1 d . . . C11 C -0.6711(3) 0.7739(2) -0.9099(4) 0.0321(10) Uani 1 1 d . . . H11A H -0.6178 0.7905 -0.8491 0.038 Uiso 1 1 calc R . . C12 C -0.7548(3) 0.7617(2) -0.8950(3) 0.0296(9) Uani 1 1 d . . . H12A H -0.7575 0.7694 -0.8238 0.036 Uiso 1 1 calc R . . C13 C 0.0319(6) 0.4532(4) -0.2059(8) 0.034(2) Uani 0.50 1 d P . . C14 C -0.0700(8) 0.5119(6) -0.3787(10) 0.065(3) Uani 0.50 1 d P . . C15 C 0.0286(10) 0.5805(5) -0.2056(11) 0.075(4) Uani 0.50 1 d P . . C16 C -0.5340(7) 0.4866(5) -1.2770(12) 0.057(4) Uani 0.50 1 d P . . C17 C -0.5839(10) 0.4070(6) -1.3563(12) 0.066(4) Uani 0.50 1 d PD . . C18 C -0.4361(13) 0.3639(8) -1.1809(15) 0.107(7) Uani 0.50 1 d PD . . O1 O -0.4271(2) 0.65137(14) -1.0199(2) 0.0336(7) Uani 1 1 d . . . O2 O -0.30457(18) 0.70861(12) -0.8935(2) 0.0246(6) Uani 1 1 d . . . O3 O -0.3086(2) 0.35193(14) -0.6868(3) 0.0373(7) Uani 1 1 d . . . O4 O -0.15908(19) 0.38667(14) -0.6053(3) 0.0377(7) Uani 1 1 d . . . O5 O -0.50043(19) 0.78812(15) -0.9430(3) 0.0375(7) Uani 1 1 d . . . O6 O -0.57331(19) 0.76734(15) -1.1297(2) 0.0345(7) Uani 1 1 d . . . O1W O -0.37797(18) 0.79720(13) -1.1196(2) 0.0227(6) Uani 1 1 d . . . H1WA H -0.3235 0.8032 -1.1228 0.043(14) Uiso 1 1 d R . . H1WB H -0.4134 0.8273 -1.1664 0.054(16) Uiso 1 1 d R . . O8 O 0.0000 0.3939(2) -0.2500 0.0432(11) Uani 1 2 d S . . O9 O -0.5000 0.5390(3) -1.2500 0.082(2) Uani 1 2 d S . . N1 N 0.0000 0.5120(3) -0.2500 0.0443(14) Uani 1 2 d S . . N2 N -0.5000 0.4214(3) -1.2500 0.0548(17) Uani 1 2 d S . . 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 0.0151(2) 0.0186(2) 0.0223(2) -0.00177(16) 0.00636(19) -0.00090(17) Ba1 0.01588(18) 0.01833(18) 0.02030(18) 0.000 0.00439(13) 0.000 C1 0.023(2) 0.025(2) 0.024(2) 0.0057(16) 0.0151(18) 0.0015(17) C2 0.0216(19) 0.0215(19) 0.0203(19) 0.0021(15) 0.0077(16) -0.0003(16) C3 0.031(2) 0.027(2) 0.022(2) 0.0043(17) -0.0002(18) -0.0046(18) C4 0.037(2) 0.022(2) 0.037(2) -0.0022(18) 0.008(2) -0.0068(19) C5 0.0209(19) 0.0200(19) 0.033(2) 0.0059(16) 0.0102(18) 0.0019(16) C6 0.021(2) 0.032(2) 0.026(2) 0.0089(17) -0.0004(18) -0.0004(17) C7 0.024(2) 0.0212(19) 0.031(2) 0.0042(16) 0.0033(18) -0.0061(17) C8 0.022(2) 0.023(2) 0.028(2) 0.0039(16) 0.0096(18) 0.0042(17) C9 0.021(2) 0.024(2) 0.037(2) -0.0008(17) 0.016(2) 0.0016(17) C10 0.0181(19) 0.028(2) 0.030(2) -0.0023(17) 0.0120(18) 0.0019(17) C11 0.020(2) 0.046(3) 0.030(2) -0.0105(19) 0.0095(18) -0.0061(19) C12 0.023(2) 0.043(2) 0.028(2) -0.0050(18) 0.0156(19) -0.0023(19) C13 0.025(4) 0.029(5) 0.049(6) 0.002(4) 0.014(4) -0.001(4) C14 0.059(7) 0.080(8) 0.043(6) 0.011(6) 0.005(6) 0.019(6) C15 0.099(13) 0.022(4) 0.111(13) -0.023(5) 0.049(10) -0.006(6) C16 0.062(8) 0.055(6) 0.087(11) -0.001(6) 0.066(9) -0.002(5) C17 0.090(10) 0.043(7) 0.080(9) -0.018(7) 0.051(8) -0.029(8) C18 0.163(17) 0.057(8) 0.151(18) 0.071(10) 0.115(14) 0.064(11) O1 0.0312(16) 0.0334(15) 0.0247(16) 0.0089(12) -0.0018(14) -0.0036(13) O2 0.0188(13) 0.0198(13) 0.0321(16) 0.0053(11) 0.0065(12) -0.0003(11) O3 0.0286(16) 0.0246(15) 0.056(2) 0.0104(14) 0.0131(15) -0.0057(13) O4 0.0242(15) 0.0266(15) 0.052(2) 0.0159(14) 0.0037(15) 0.0011(12) O5 0.0209(15) 0.0531(19) 0.0434(19) -0.0146(15) 0.0179(15) -0.0108(14) O6 0.0266(15) 0.0493(18) 0.0351(17) 0.0032(14) 0.0200(14) 0.0033(14) O1W 0.0178(13) 0.0283(14) 0.0236(14) 0.0050(11) 0.0096(12) -0.0016(12) O8 0.053(3) 0.018(2) 0.047(3) 0.000 0.006(2) 0.000 O9 0.077(4) 0.026(3) 0.170(7) 0.000 0.078(5) 0.000 N1 0.050(3) 0.023(3) 0.064(4) 0.000 0.026(3) 0.000 N2 0.083(5) 0.029(3) 0.076(5) 0.000 0.057(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.939(3) . ? Zn1 O4 1.957(3) 4_453 ? Zn1 O2 1.976(2) . ? Zn1 O1W 2.010(2) . ? Ba1 O9 2.694(5) . ? Ba1 O1 2.743(3) . ? Ba1 O1 2.743(3) 2_452 ? Ba1 O6 2.760(3) . ? Ba1 O6 2.760(3) 2_452 ? Ba1 O3 2.764(3) 6_565 ? Ba1 O3 2.764(3) 5_463 ? Ba1 O1W 2.959(2) . ? Ba1 O1W 2.959(2) 2_452 ? C1 O1 1.230(5) . ? C1 O2 1.290(4) . ? C1 C2 1.495(5) . ? C2 C7 1.387(5) . ? C2 C3 1.394(5) . ? C3 C4 1.381(5) . ? C3 H3A 0.9300 . ? C4 C5 1.385(5) . ? C4 H4A 0.9300 . ? C5 C6 1.381(5) . ? C5 C8 1.507(5) . ? C6 C7 1.389(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 O3 1.223(4) . ? C8 O4 1.263(5) . ? C9 O6 1.234(5) . ? C9 O5 1.278(5) . ? C9 C10 1.508(5) . ? C10 C12 1.373(5) 7_363 ? C10 C11 1.390(5) . ? C11 C12 1.373(5) . ? C11 H11A 0.9300 . ? C12 C10 1.373(5) 7_363 ? C12 H12A 0.9300 . ? C13 C13 1.160(17) 2_554 ? C13 N1 1.262(9) . ? C13 O8 1.270(8) . ? C13 C14 1.503(13) 2_554 ? C14 C13 1.503(13) 2_554 ? C14 N1 1.564(11) . ? C14 C15 1.651(16) 2_554 ? C15 C15 1.12(2) 2_554 ? C15 N1 1.421(10) . ? C15 C14 1.651(16) 2_554 ? C16 C16 0.99(2) 2_452 ? C16 O9 1.115(10) . ? C16 N2 1.338(11) . ? C16 C17 1.816(17) . ? C17 C18 0.94(2) 2_452 ? C17 N2 1.477(15) . ? C18 C17 0.94(2) 2_452 ? C18 N2 1.501(13) . ? O3 Ba1 2.764(3) 5_463 ? O4 Zn1 1.957(3) 4_443 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O8 C13 1.270(8) 2_554 ? O9 C16 1.115(10) 2_452 ? N1 C13 1.262(9) 2_554 ? N1 C15 1.421(10) 2_554 ? N1 C14 1.564(11) 2_554 ? N2 C16 1.338(11) 2_452 ? N2 C17 1.477(15) 2_452 ? N2 C18 1.501(14) 2_452 ? 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 O5 Zn1 O4 97.72(12) . 4_453 ? O5 Zn1 O2 108.29(12) . . ? O4 Zn1 O2 121.92(12) 4_453 . ? O5 Zn1 O1W 119.94(12) . . ? O4 Zn1 O1W 106.48(12) 4_453 . ? O2 Zn1 O1W 103.67(11) . . ? O9 Ba1 O1 78.41(6) . . ? O9 Ba1 O1 78.41(6) . 2_452 ? O1 Ba1 O1 156.82(12) . 2_452 ? O9 Ba1 O6 126.96(6) . . ? O1 Ba1 O6 67.51(9) . . ? O1 Ba1 O6 128.62(8) 2_452 . ? O9 Ba1 O6 126.96(6) . 2_452 ? O1 Ba1 O6 128.62(8) . 2_452 ? O1 Ba1 O6 67.51(8) 2_452 2_452 ? O6 Ba1 O6 106.09(12) . 2_452 ? O9 Ba1 O3 77.16(6) . 6_565 ? O1 Ba1 O3 72.63(9) . 6_565 ? O1 Ba1 O3 102.08(9) 2_452 6_565 ? O6 Ba1 O3 125.15(8) . 6_565 ? O6 Ba1 O3 72.03(9) 2_452 6_565 ? O9 Ba1 O3 77.16(6) . 5_463 ? O1 Ba1 O3 102.08(9) . 5_463 ? O1 Ba1 O3 72.63(9) 2_452 5_463 ? O6 Ba1 O3 72.03(9) . 5_463 ? O6 Ba1 O3 125.15(8) 2_452 5_463 ? O3 Ba1 O3 154.32(11) 6_565 5_463 ? O9 Ba1 O1W 138.88(5) . . ? O1 Ba1 O1W 69.55(7) . . ? O1 Ba1 O1W 130.70(8) 2_452 . ? O6 Ba1 O1W 62.46(8) . . ? O6 Ba1 O1W 63.68(8) 2_452 . ? O3 Ba1 O1W 69.27(7) 6_565 . ? O3 Ba1 O1W 133.53(8) 5_463 . ? O9 Ba1 O1W 138.88(5) . 2_452 ? O1 Ba1 O1W 130.70(8) . 2_452 ? O1 Ba1 O1W 69.55(7) 2_452 2_452 ? O6 Ba1 O1W 63.68(8) . 2_452 ? O6 Ba1 O1W 62.46(8) 2_452 2_452 ? O3 Ba1 O1W 133.53(8) 6_565 2_452 ? O3 Ba1 O1W 69.27(7) 5_463 2_452 ? O1W Ba1 O1W 82.24(10) . 2_452 ? O1 C1 O2 122.9(3) . . ? O1 C1 C2 119.8(3) . . ? O2 C1 C2 117.2(3) . . ? C7 C2 C3 119.1(3) . . ? C7 C2 C1 122.7(3) . . ? C3 C2 C1 118.1(3) . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 119.2(3) . . ? C6 C5 C8 121.7(4) . . ? C4 C5 C8 119.1(3) . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H6A 119.6 . . ? C7 C6 H6A 119.6 . . ? C2 C7 C6 120.0(4) . . ? C2 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? O3 C8 O4 124.3(4) . . ? O3 C8 C5 120.2(3) . . ? O4 C8 C5 115.5(3) . . ? O6 C9 O5 124.5(3) . . ? O6 C9 C10 119.6(4) . . ? O5 C9 C10 115.9(3) . . ? C12 C10 C11 119.2(3) 7_363 . ? C12 C10 C9 119.5(3) 7_363 . ? C11 C10 C9 121.3(4) . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C10 120.4(4) . 7_363 ? C11 C12 H12A 119.8 . . ? C10 C12 H12A 119.8 7_363 . ? C13 C13 N1 62.6(4) 2_554 . ? C13 C13 O8 62.8(4) 2_554 . ? N1 C13 O8 125.5(7) . . ? C13 C13 C14 129.3(6) 2_554 2_554 ? N1 C13 C14 68.2(6) . 2_554 ? O8 C13 C14 162.3(9) . 2_554 ? C13 C14 N1 48.6(5) 2_554 . ? C13 C14 C15 100.6(8) 2_554 2_554 ? N1 C14 C15 52.4(6) . 2_554 ? C15 C15 N1 66.8(5) 2_554 . ? C15 C15 C14 126.9(6) 2_554 2_554 ? N1 C15 C14 60.6(5) . 2_554 ? C16 C16 O9 63.5(6) 2_452 . ? C16 C16 N2 68.2(5) 2_452 . ? O9 C16 N2 131.7(10) . . ? C16 C16 C17 118.7(7) 2_452 . ? O9 C16 C17 164.3(11) . . ? N2 C16 C17 53.3(6) . . ? C18 C17 N2 73.0(17) 2_452 . ? C18 C17 C16 118.1(19) 2_452 . ? N2 C17 C16 46.6(6) . . ? C17 C18 N2 70.3(12) 2_452 . ? C1 O1 Ba1 142.9(2) . . ? C1 O2 Zn1 111.7(2) . . ? C8 O3 Ba1 150.7(2) . 5_463 ? C8 O4 Zn1 117.5(2) . 4_443 ? C9 O5 Zn1 116.2(2) . . ? C9 O6 Ba1 139.8(3) . . ? Zn1 O1W Ba1 106.47(9) . . ? Zn1 O1W H1WA 116.0 . . ? Ba1 O1W H1WA 119.0 . . ? Zn1 O1W H1WB 117.9 . . ? Ba1 O1W H1WB 91.7 . . ? H1WA O1W H1WB 103.9 . . ? C13 O8 C13 54.4(8) . 2_554 ? C16 O9 C16 52.9(12) . 2_452 ? C16 O9 Ba1 153.5(6) . . ? C16 O9 Ba1 153.5(6) 2_452 . ? C13 N1 C13 54.7(8) . 2_554 ? C13 N1 C15 129.4(6) . . ? C13 N1 C15 175.4(7) 2_554 . ? C13 N1 C15 175.4(7) . 2_554 ? C13 N1 C15 129.4(6) 2_554 2_554 ? C15 N1 C15 46.5(10) . 2_554 ? C13 N1 C14 63.2(6) . 2_554 ? C13 N1 C14 116.7(7) 2_554 2_554 ? C15 N1 C14 66.9(7) . 2_554 ? C15 N1 C14 113.1(8) 2_554 2_554 ? C13 N1 C14 116.7(7) . . ? C13 N1 C14 63.2(6) 2_554 . ? C15 N1 C14 113.1(8) . . ? C15 N1 C14 66.9(7) 2_554 . ? C14 N1 C14 179.9(10) 2_554 . ? C16 N2 C16 43.6(10) 2_452 . ? C16 N2 C17 80.1(7) 2_452 2_452 ? C16 N2 C17 121.1(8) . 2_452 ? C16 N2 C17 121.1(8) 2_452 . ? C16 N2 C17 80.1(7) . . ? C17 N2 C17 158.5(11) 2_452 . ? C16 N2 C18 115.6(9) 2_452 . ? C16 N2 C18 157.8(10) . . ? C17 N2 C18 36.7(8) 2_452 . ? C17 N2 C18 122.0(10) . . ? C16 N2 C18 157.8(10) 2_452 2_452 ? C16 N2 C18 115.6(9) . 2_452 ? C17 N2 C18 122.0(10) 2_452 2_452 ? C17 N2 C18 36.7(8) . 2_452 ? C18 N2 C18 86.1(15) . 2_452 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.475 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.084 #=========================END