# Electronic Supplementary MAterial for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ning-Hai Hu' _publ_contact_author_email HUNH@CIAC.JL.CN _publ_section_title ; Construction of coordination networks with high connectivity: a new 8-connected self-penetrating network based on tetranuclear metal clusters ; loop_ _publ_author_name 'Ning-Hai Hu.' 'Stuart Batten' 'Heng-Quing Jia.' 'Zhi-Gang Li.' 'Guan-Hua Wang.' ; Jing-Wei Xu ; # Attachment 'ccdc_681826_681827_cif.txt' data_l082 _database_code_depnum_ccdc_archive 'CCDC 681826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Co4 (C7 H3 N O4)4 (C12 H10 N2)' _chemical_formula_sum 'C40 H22 Co4 N6 O16' _chemical_formula_weight 1078.36 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' Co Co 0.3494 0.9721 '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 22.7592(18) _cell_length_b 11.3409(9) _cell_length_c 17.5006(13) _cell_angle_alpha 90.00 _cell_angle_beta 113.104(1) _cell_angle_gamma 90.00 _cell_volume 4154.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used 5884 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.03 _exptl_crystal_description column _exptl_crystal_colour dark-pink _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6659 _exptl_absorpt_correction_T_max 0.9294 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _diffrn_ambient_temperature 187(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 APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11388 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4093 _reflns_number_gt 3690 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2007)' _computing_publication_material SHELXTL _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^)+(0.0376P)^2^+3.8340P] 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 4093 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _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 Co1 Co 0.101733(12) 0.25635(2) 0.019779(15) 0.01564(8) Uani 1 1 d . . . Co2 Co 0.105256(12) 0.50429(2) 0.135442(14) 0.01453(8) Uani 1 1 d . . . O1 O 0.06953(9) 0.84596(13) -0.34887(9) 0.0377(4) Uani 1 1 d . . . O2 O 0.07018(6) 0.66592(12) -0.39962(8) 0.0201(3) Uani 1 1 d . . . O3 O 0.12382(6) 0.38654(12) -0.04058(8) 0.0215(3) Uani 1 1 d . . . O4 O 0.10913(7) 0.55101(12) 0.02198(8) 0.0227(3) Uani 1 1 d . . . O5 O 0.47969(6) 0.10104(11) 0.40538(8) 0.0213(3) Uani 1 1 d . . . O6 O 0.51550(6) 0.28736(12) 0.43271(8) 0.0226(3) Uani 1 1 d . . . O7 O 0.19364(7) 0.26770(12) 0.12336(9) 0.0266(3) Uani 1 1 d . . . O8 O 0.19899(6) 0.44569(12) 0.18265(8) 0.0218(3) Uani 1 1 d . . . N1 N 0.09415(8) 0.56384(14) -0.25603(9) 0.0194(3) Uani 1 1 d . . . N2 N 0.36257(7) 0.17355(14) 0.31469(9) 0.0164(3) Uani 1 1 d . . . N3 N 0.14427(8) 0.10717(14) -0.00269(10) 0.0198(3) Uani 1 1 d . . . C1 C 0.07259(10) 0.73878(17) -0.34129(12) 0.0220(4) Uani 1 1 d . . . C2 C 0.08142(10) 0.68036(17) -0.26007(12) 0.0207(4) Uani 1 1 d . . . C3 C 0.07700(11) 0.74269(18) -0.19471(13) 0.0273(5) Uani 1 1 d . . . H3 H 0.0683 0.8249 -0.1994 0.033 Uiso 1 1 calc R . . C4 C 0.08556(11) 0.68242(18) -0.12201(12) 0.0258(5) Uani 1 1 d . . . H4 H 0.0818 0.7226 -0.0765 0.031 Uiso 1 1 calc R . . C5 C 0.09970(9) 0.56304(18) -0.11652(11) 0.0198(4) Uani 1 1 d . . . C6 C 0.10322(10) 0.50753(17) -0.18541(12) 0.0215(4) Uani 1 1 d . . . H6 H 0.1125 0.4256 -0.1820 0.026 Uiso 1 1 calc R . . C7 C 0.11126(9) 0.49467(16) -0.03828(12) 0.0183(4) Uani 1 1 d . . . C8 C 0.47320(9) 0.21101(17) 0.39786(11) 0.0178(4) Uani 1 1 d . . . C9 C 0.40836(9) 0.25669(16) 0.34066(11) 0.0170(4) Uani 1 1 d . . . C10 C 0.39683(9) 0.37343(17) 0.31665(12) 0.0215(4) Uani 1 1 d . . . H10 H 0.4301 0.4302 0.3355 0.026 Uiso 1 1 calc R . . C11 C 0.33517(10) 0.40547(17) 0.26410(12) 0.0227(4) Uani 1 1 d . . . H11 H 0.3254 0.4856 0.2484 0.027 Uiso 1 1 calc R . . C12 C 0.28810(9) 0.31996(16) 0.23480(11) 0.0178(4) Uani 1 1 d . . . C13 C 0.30425(9) 0.20438(17) 0.26161(11) 0.0182(4) Uani 1 1 d . . . H13 H 0.2724 0.1450 0.2413 0.022 Uiso 1 1 calc R . . C14 C 0.22092(9) 0.34670(17) 0.17505(11) 0.0184(4) Uani 1 1 d . . . C15 C 0.13297(11) 0.00231(18) 0.02385(15) 0.0289(5) Uani 1 1 d . . . H15 H 0.1002 -0.0030 0.0445 0.035 Uiso 1 1 calc R . . C16 C 0.16654(11) -0.09839(18) 0.02274(15) 0.0315(5) Uani 1 1 d . . . H16 H 0.1577 -0.1703 0.0440 0.038 Uiso 1 1 calc R . . C17 C 0.21357(10) -0.09399(17) -0.00975(12) 0.0223(4) Uani 1 1 d . . . C18 C 0.22387(10) 0.01400(18) -0.03926(14) 0.0265(5) Uani 1 1 d . . . H18 H 0.2546 0.0209 -0.0633 0.032 Uiso 1 1 calc R . . C19 C 0.18948(10) 0.11182(18) -0.03372(13) 0.0260(5) Uani 1 1 d . . . H19 H 0.1983 0.1855 -0.0528 0.031 Uiso 1 1 calc R . . C20 C 0.25132(10) -0.19640(18) -0.01463(13) 0.0269(5) Uani 1 1 d . . . H20 H 0.2802 -0.1851 -0.0411 0.032 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 Co1 0.01429(14) 0.01396(14) 0.01631(13) -0.00215(9) 0.00346(11) 0.00206(10) Co2 0.01454(14) 0.01379(14) 0.01385(13) -0.00114(9) 0.00405(11) 0.00087(9) O1 0.0653(12) 0.0187(8) 0.0326(8) 0.0063(6) 0.0230(8) 0.0042(8) O2 0.0230(7) 0.0194(7) 0.0182(6) 0.0030(5) 0.0085(6) 0.0042(6) O3 0.0217(7) 0.0212(7) 0.0239(7) 0.0039(6) 0.0114(6) 0.0025(6) O4 0.0298(8) 0.0222(7) 0.0167(6) 0.0015(5) 0.0098(6) -0.0001(6) O5 0.0150(7) 0.0192(7) 0.0250(7) 0.0034(6) 0.0028(6) -0.0008(5) O6 0.0161(7) 0.0193(7) 0.0244(7) 0.0039(6) -0.0008(6) -0.0038(6) O7 0.0197(8) 0.0232(7) 0.0255(7) -0.0067(6) -0.0034(6) 0.0057(6) O8 0.0161(7) 0.0175(7) 0.0267(7) -0.0019(6) 0.0032(6) 0.0035(5) N1 0.0216(9) 0.0187(8) 0.0177(8) 0.0008(6) 0.0077(7) -0.0001(7) N2 0.0142(8) 0.0153(8) 0.0169(7) 0.0012(6) 0.0030(6) 0.0003(6) N3 0.0182(8) 0.0177(8) 0.0209(8) -0.0027(6) 0.0048(7) 0.0030(7) C1 0.0251(11) 0.0210(10) 0.0220(10) 0.0034(8) 0.0113(9) 0.0034(8) C2 0.0239(11) 0.0188(10) 0.0194(9) 0.0017(8) 0.0086(8) 0.0005(8) C3 0.0419(14) 0.0167(10) 0.0265(10) 0.0017(8) 0.0168(10) 0.0058(9) C4 0.0363(12) 0.0240(11) 0.0191(9) -0.0022(8) 0.0131(9) 0.0017(9) C5 0.0187(10) 0.0227(10) 0.0177(9) -0.0001(7) 0.0066(8) -0.0005(8) C6 0.0256(11) 0.0182(10) 0.0212(9) 0.0028(7) 0.0097(9) 0.0009(8) C7 0.0148(9) 0.0212(10) 0.0184(9) 0.0001(7) 0.0060(8) -0.0028(7) C8 0.0158(10) 0.0209(10) 0.0159(8) 0.0026(7) 0.0053(8) -0.0009(8) C9 0.0150(10) 0.0182(10) 0.0162(8) -0.0001(7) 0.0047(8) -0.0021(7) C10 0.0191(10) 0.0165(10) 0.0247(10) -0.0002(8) 0.0041(8) -0.0030(8) C11 0.0232(11) 0.0146(9) 0.0258(10) 0.0015(8) 0.0046(9) 0.0015(8) C12 0.0152(9) 0.0190(9) 0.0172(8) -0.0008(7) 0.0044(8) 0.0020(8) C13 0.0140(9) 0.0190(9) 0.0191(9) -0.0008(7) 0.0038(8) -0.0017(7) C14 0.0162(10) 0.0199(10) 0.0174(9) 0.0025(7) 0.0049(8) 0.0018(8) C15 0.0323(12) 0.0228(11) 0.0404(12) 0.0027(9) 0.0239(11) 0.0059(9) C16 0.0398(13) 0.0171(10) 0.0461(13) 0.0047(9) 0.0261(11) 0.0036(9) C17 0.0214(10) 0.0193(10) 0.0251(10) -0.0023(8) 0.0079(9) 0.0035(8) C18 0.0224(11) 0.0256(11) 0.0350(12) 0.0010(9) 0.0151(10) 0.0034(9) C19 0.0254(11) 0.0202(10) 0.0342(11) 0.0015(9) 0.0137(10) 0.0018(9) C20 0.0257(12) 0.0239(11) 0.0346(11) -0.0009(9) 0.0154(10) 0.0042(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.9914(13) . ? Co1 O2 2.0192(13) 6_566 ? Co1 O6 2.0180(13) 8_455 ? Co1 N3 2.0622(16) . ? Co1 O7 2.1684(14) . ? Co2 O8 2.0717(13) . ? Co2 O2 2.0869(13) 6_566 ? Co2 O4 2.0902(13) . ? Co2 O5 2.0900(13) 4 ? Co2 N2 2.1168(15) 4 ? Co2 N1 2.1552(16) 6_566 ? O1 C1 1.222(2) . ? O2 C1 1.298(2) . ? O3 C7 1.263(2) . ? O4 C7 1.250(2) . ? O5 C8 1.257(2) . ? O6 C8 1.260(2) . ? O7 C14 1.251(2) . ? O8 C14 1.257(2) . ? N1 C6 1.333(2) . ? N1 C2 1.349(2) . ? N2 C13 1.334(2) . ? N2 C9 1.345(2) . ? N3 C15 1.338(3) . ? N3 C19 1.340(3) . ? C1 C2 1.508(3) . ? C2 C3 1.382(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.390(3) . ? C5 C7 1.504(3) . ? C6 H6 0.9500 . ? C8 C9 1.513(3) . ? C9 C10 1.383(3) . ? C10 C11 1.391(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 C13 1.392(3) . ? C12 C14 1.506(3) . ? C13 H13 0.9500 . ? C15 C16 1.378(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 H16 0.9500 . ? C17 C18 1.384(3) . ? C17 C20 1.467(3) . ? C18 C19 1.383(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C20 1.330(4) 7_545 ? C20 H20 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 O3 Co1 O2 106.25(5) . 6_566 ? O3 Co1 O6 98.90(6) . 8_455 ? O2 Co1 O6 97.33(6) 6_566 8_455 ? O3 Co1 N3 105.78(6) . . ? O2 Co1 N3 144.45(6) 6_566 . ? O6 Co1 N3 92.57(6) 8_455 . ? O3 Co1 O7 92.17(6) . . ? O2 Co1 O7 83.16(5) 6_566 . ? O6 Co1 O7 168.27(6) 8_455 . ? N3 Co1 O7 80.62(6) . . ? O8 Co2 O2 92.05(5) . 6_566 ? O8 Co2 O4 92.26(6) . . ? O2 Co2 O4 96.26(5) 6_566 . ? O8 Co2 O5 167.00(5) . 4 ? O2 Co2 O5 100.91(5) 6_566 4 ? O4 Co2 O5 85.43(6) . 4 ? O8 Co2 N2 89.49(6) . 4 ? O2 Co2 N2 172.08(5) 6_566 4 ? O4 Co2 N2 91.44(6) . 4 ? O5 Co2 N2 77.80(6) 4 4 ? O8 Co2 N1 89.55(6) . 6_566 ? O2 Co2 N1 76.35(5) 6_566 6_566 ? O4 Co2 N1 172.45(6) . 6_566 ? O5 Co2 N1 94.40(6) 4 6_566 ? N2 Co2 N1 95.91(6) 4 6_566 ? C1 O2 Co1 110.78(12) . 6_565 ? C1 O2 Co2 117.67(11) . 6_565 ? Co1 O2 Co2 114.16(6) 6_565 6_565 ? C7 O3 Co1 126.54(12) . . ? C7 O4 Co2 134.57(13) . . ? C8 O5 Co2 115.50(12) . 4_545 ? C8 O6 Co1 121.92(12) . 8_556 ? C14 O7 Co1 133.56(13) . . ? C14 O8 Co2 129.35(13) . . ? C6 N1 C2 118.02(16) . . ? C6 N1 Co2 128.04(13) . 6_565 ? C2 N1 Co2 113.71(12) . 6_565 ? C13 N2 C9 118.60(16) . . ? C13 N2 Co2 127.84(13) . 4_545 ? C9 N2 Co2 113.55(12) . 4_545 ? C15 N3 C19 117.30(17) . . ? C15 N3 Co1 119.63(14) . . ? C19 N3 Co1 122.53(14) . . ? O1 C1 O2 124.41(18) . . ? O1 C1 C2 121.34(18) . . ? O2 C1 C2 114.23(16) . . ? N1 C2 C3 122.81(17) . . ? N1 C2 C1 115.23(16) . . ? C3 C2 C1 121.96(18) . . ? C2 C3 C4 118.49(18) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.30(18) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 118.23(17) . . ? C4 C5 C7 121.29(17) . . ? C6 C5 C7 120.47(18) . . ? N1 C6 C5 123.12(18) . . ? N1 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? O4 C7 O3 127.39(18) . . ? O4 C7 C5 116.97(17) . . ? O3 C7 C5 115.60(16) . . ? O5 C8 O6 126.53(18) . . ? O5 C8 C9 116.94(16) . . ? O6 C8 C9 116.53(17) . . ? N2 C9 C10 122.62(18) . . ? N2 C9 C8 114.12(16) . . ? C10 C9 C8 123.25(17) . . ? C9 C10 C11 118.22(18) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C12 C11 C10 119.66(18) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 118.08(17) . . ? C11 C12 C14 122.88(17) . . ? C13 C12 C14 119.04(17) . . ? N2 C13 C12 122.72(17) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? O7 C14 O8 127.67(18) . . ? O7 C14 C12 116.00(17) . . ? O8 C14 C12 116.33(16) . . ? N3 C15 C16 123.3(2) . . ? N3 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C17 119.6(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 116.91(18) . . ? C18 C17 C20 119.33(19) . . ? C16 C17 C20 123.75(19) . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? N3 C19 C18 122.9(2) . . ? N3 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C20 C20 C17 125.8(3) 7_545 . ? C20 C20 H20 117.1 7_545 . ? C17 C20 H20 117.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.407 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.065 data_l002 _database_code_depnum_ccdc_archive 'CCDC 681827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn4 (C7 H3 N O4)4 (C12 H10 N2)' _chemical_formula_sum 'C40 H22 N6 O16 Zn4' _chemical_formula_weight 1104.12 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' _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 22.536(3) _cell_length_b 11.3199(13) _cell_length_c 17.570(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.339(2) _cell_angle_gamma 90.00 _cell_volume 4145.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used 2347 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4785 _exptl_absorpt_correction_T_max 0.7993 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _diffrn_ambient_temperature 187(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 APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11823 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.06 _reflns_number_total 4091 _reflns_number_gt 3242 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2007)' _computing_publication_material SHELXTL _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^)+(0.0385P)^2^] 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 4091 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.103463(19) 0.25951(3) 0.01980(2) 0.01466(11) Uani 1 1 d . . . Zn2 Zn 0.105301(18) 0.50410(3) 0.13275(2) 0.01395(11) Uani 1 1 d . . . O1 O 0.07012(14) 0.8472(2) -0.34695(16) 0.0329(7) Uani 1 1 d . . . O2 O 0.07077(11) 0.66793(19) -0.39967(14) 0.0162(5) Uani 1 1 d . . . O3 O 0.12431(11) 0.38303(19) -0.04473(15) 0.0194(6) Uani 1 1 d . . . O4 O 0.11015(11) 0.5467(2) 0.01960(14) 0.0207(6) Uani 1 1 d . . . O5 O 0.48048(11) 0.10077(19) 0.40948(15) 0.0196(5) Uani 1 1 d . . . O6 O 0.51613(11) 0.2875(2) 0.43477(15) 0.0215(6) Uani 1 1 d . . . O7 O 0.19606(12) 0.2692(2) 0.12447(16) 0.0260(6) Uani 1 1 d . . . O8 O 0.20160(11) 0.44863(19) 0.18095(15) 0.0208(6) Uani 1 1 d . . . N1 N 0.09475(14) 0.5636(2) -0.25698(18) 0.0178(6) Uani 1 1 d . . . N2 N 0.36304(13) 0.1739(2) 0.31581(17) 0.0145(6) Uani 1 1 d . . . N3 N 0.14343(13) 0.1073(2) -0.00116(18) 0.0173(6) Uani 1 1 d . . . C1 C 0.07327(17) 0.7396(3) -0.3409(2) 0.0192(8) Uani 1 1 d . . . C2 C 0.08205(16) 0.6806(3) -0.2606(2) 0.0175(8) Uani 1 1 d . . . C3 C 0.07763(18) 0.7418(3) -0.1949(2) 0.0240(9) Uani 1 1 d . . . H3 H 0.0690 0.8242 -0.1991 0.029 Uiso 1 1 calc R . . C4 C 0.08600(17) 0.6815(3) -0.1230(2) 0.0220(8) Uani 1 1 d . . . H4 H 0.0822 0.7215 -0.0776 0.026 Uiso 1 1 calc R . . C5 C 0.10012(16) 0.5612(3) -0.1183(2) 0.0166(8) Uani 1 1 d . . . C6 C 0.10358(16) 0.5068(3) -0.1871(2) 0.0187(8) Uani 1 1 d . . . H6 H 0.1127 0.4246 -0.1843 0.022 Uiso 1 1 calc R . . C7 C 0.11186(16) 0.4920(3) -0.0413(2) 0.0173(8) Uani 1 1 d . . . C8 C 0.47377(17) 0.2107(3) 0.4004(2) 0.0155(7) Uani 1 1 d . . . C9 C 0.40947(16) 0.2562(3) 0.3417(2) 0.0152(7) Uani 1 1 d . . . C10 C 0.39907(17) 0.3726(3) 0.3168(2) 0.0191(8) Uani 1 1 d . . . H10 H 0.4329 0.4287 0.3354 0.023 Uiso 1 1 calc R . . C11 C 0.33793(17) 0.4057(3) 0.2640(2) 0.0203(8) Uani 1 1 d . . . H11 H 0.3290 0.4858 0.2477 0.024 Uiso 1 1 calc R . . C12 C 0.29016(16) 0.3213(3) 0.2354(2) 0.0159(7) Uani 1 1 d . . . C13 C 0.30515(16) 0.2054(3) 0.2627(2) 0.0171(8) Uani 1 1 d . . . H13 H 0.2728 0.1466 0.2427 0.021 Uiso 1 1 calc R . . C14 C 0.22324(17) 0.3486(3) 0.1749(2) 0.0175(8) Uani 1 1 d . . . C15 C 0.13247(19) 0.0029(3) 0.0261(3) 0.0269(9) Uani 1 1 d . . . H15 H 0.1001 -0.0020 0.0481 0.032 Uiso 1 1 calc R . . C16 C 0.16574(19) -0.0982(3) 0.0238(3) 0.0280(9) Uani 1 1 d . . . H16 H 0.1567 -0.1704 0.0448 0.034 Uiso 1 1 calc R . . C17 C 0.21271(17) -0.0940(3) -0.0095(2) 0.0211(8) Uani 1 1 d . . . C18 C 0.22325(18) 0.0139(3) -0.0390(2) 0.0250(9) Uani 1 1 d . . . H18 H 0.2543 0.0210 -0.0632 0.030 Uiso 1 1 calc R . . C19 C 0.18851(17) 0.1111(3) -0.0330(2) 0.0229(8) Uani 1 1 d . . . H19 H 0.1971 0.1847 -0.0527 0.028 Uiso 1 1 calc R . . C20 C 0.25116(18) -0.1965(3) -0.0148(2) 0.0240(9) Uani 1 1 d . . . H20 H 0.2801 -0.1851 -0.0418 0.029 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 Zn1 0.0155(2) 0.0123(2) 0.0141(2) -0.00098(17) 0.00334(17) 0.00231(17) Zn2 0.0161(2) 0.0115(2) 0.0131(2) -0.00081(16) 0.00418(17) 0.00094(16) O1 0.061(2) 0.0134(13) 0.0279(16) 0.0034(12) 0.0214(15) 0.0008(13) O2 0.0207(14) 0.0151(12) 0.0130(13) 0.0009(10) 0.0067(11) 0.0005(10) O3 0.0240(14) 0.0153(13) 0.0207(14) 0.0044(11) 0.0106(12) 0.0022(10) O4 0.0272(15) 0.0202(12) 0.0141(13) 0.0013(11) 0.0071(11) 0.0004(11) O5 0.0135(13) 0.0159(12) 0.0245(14) 0.0024(11) 0.0017(11) 0.0003(10) O6 0.0167(14) 0.0171(12) 0.0233(14) 0.0022(11) -0.0008(11) -0.0036(11) O7 0.0210(15) 0.0209(13) 0.0247(15) -0.0075(12) -0.0043(12) 0.0061(11) O8 0.0176(14) 0.0134(12) 0.0267(15) 0.0006(11) 0.0033(11) 0.0051(10) N1 0.0211(17) 0.0147(15) 0.0183(17) 0.0013(13) 0.0081(13) 0.0009(13) N2 0.0141(15) 0.0145(14) 0.0126(15) 0.0002(12) 0.0025(12) 0.0003(12) N3 0.0160(16) 0.0181(15) 0.0167(16) -0.0017(13) 0.0051(13) 0.0016(12) C1 0.021(2) 0.0169(19) 0.020(2) 0.0036(16) 0.0082(16) -0.0002(15) C2 0.0164(19) 0.0190(18) 0.017(2) 0.0023(15) 0.0065(16) 0.0022(15) C3 0.035(2) 0.0121(17) 0.025(2) 0.0007(16) 0.0109(19) 0.0043(16) C4 0.030(2) 0.0190(19) 0.018(2) -0.0035(16) 0.0094(18) 0.0006(16) C5 0.0130(19) 0.0146(17) 0.022(2) 0.0001(15) 0.0067(16) -0.0017(14) C6 0.022(2) 0.0157(17) 0.019(2) 0.0024(15) 0.0083(16) -0.0031(15) C7 0.0124(18) 0.0211(19) 0.018(2) 0.0017(16) 0.0049(15) -0.0035(15) C8 0.0193(19) 0.0148(17) 0.0122(18) 0.0028(15) 0.0058(15) -0.0013(15) C9 0.0145(18) 0.0135(17) 0.0150(18) 0.0000(15) 0.0027(15) -0.0013(14) C10 0.019(2) 0.0156(18) 0.019(2) -0.0008(15) 0.0030(16) -0.0057(15) C11 0.023(2) 0.0152(17) 0.022(2) 0.0014(16) 0.0077(17) 0.0033(15) C12 0.0135(18) 0.0170(17) 0.0154(19) -0.0004(15) 0.0036(15) 0.0029(14) C13 0.0132(19) 0.0193(18) 0.0164(19) -0.0009(15) 0.0029(16) -0.0026(15) C14 0.0177(19) 0.0196(18) 0.0149(19) 0.0046(16) 0.0058(16) 0.0014(15) C15 0.030(2) 0.023(2) 0.037(2) 0.0046(18) 0.022(2) 0.0053(17) C16 0.036(2) 0.0137(18) 0.042(3) 0.0039(18) 0.023(2) 0.0035(17) C17 0.019(2) 0.0187(18) 0.026(2) -0.0027(16) 0.0091(17) 0.0030(15) C18 0.024(2) 0.022(2) 0.035(2) 0.0011(17) 0.0173(19) -0.0011(16) C19 0.024(2) 0.0176(19) 0.028(2) 0.0045(16) 0.0103(18) 0.0000(16) C20 0.023(2) 0.0198(18) 0.030(2) 0.0025(17) 0.0113(18) 0.0063(16) 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 O3 1.966(2) . ? Zn1 O2 2.003(2) 6_566 ? Zn1 O6 2.038(2) 8_455 ? Zn1 N3 2.042(3) . ? Zn1 O7 2.198(2) . ? Zn2 O4 2.088(2) . ? Zn2 O2 2.094(2) 6_566 ? Zn2 O5 2.096(2) 4 ? Zn2 O8 2.103(2) . ? Zn2 N2 2.128(3) 4 ? Zn2 N1 2.179(3) 6_566 ? O1 C1 1.223(4) . ? O2 C1 1.297(4) . ? O3 C7 1.271(4) . ? O4 C7 1.250(4) . ? O5 C8 1.256(4) . ? O6 C8 1.262(4) . ? O7 C14 1.248(4) . ? O8 C14 1.253(4) . ? N1 C6 1.333(4) . ? N1 C2 1.351(4) . ? N2 C13 1.332(4) . ? N2 C9 1.345(4) . ? N3 C15 1.332(4) . ? N3 C19 1.334(4) . ? C1 C2 1.505(5) . ? C2 C3 1.382(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.385(5) . ? C5 C7 1.497(5) . ? C6 H6 0.9500 . ? C8 C9 1.514(5) . ? C9 C10 1.379(4) . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 C13 1.395(4) . ? C12 C14 1.510(5) . ? C13 H13 0.9500 . ? C15 C16 1.377(5) . ? C15 H15 0.9500 . ? C16 C17 1.391(5) . ? C16 H16 0.9500 . ? C17 C18 1.382(5) . ? C17 C20 1.472(4) . ? C18 C19 1.377(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C20 1.327(7) 7_545 ? C20 H20 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 O3 Zn1 O2 110.39(9) . 6_566 ? O3 Zn1 O6 97.97(10) . 8_455 ? O2 Zn1 O6 96.48(9) 6_566 8_455 ? O3 Zn1 N3 106.12(10) . . ? O2 Zn1 N3 141.22(10) 6_566 . ? O6 Zn1 N3 90.96(10) 8_455 . ? O3 Zn1 O7 95.05(10) . . ? O2 Zn1 O7 82.86(9) 6_566 . ? O6 Zn1 O7 166.31(9) 8_455 . ? N3 Zn1 O7 81.34(10) . . ? O4 Zn2 O2 96.00(9) . 6_566 ? O4 Zn2 O5 85.26(9) . 4 ? O2 Zn2 O5 101.05(9) 6_566 4 ? O4 Zn2 O8 91.89(9) . . ? O2 Zn2 O8 92.97(9) 6_566 . ? O5 Zn2 O8 165.90(9) 4 . ? O4 Zn2 N2 93.74(9) . 4 ? O2 Zn2 N2 170.13(9) 6_566 4 ? O5 Zn2 N2 78.12(9) 4 4 ? O8 Zn2 N2 88.31(10) . 4 ? O4 Zn2 N1 172.09(9) . 6_566 ? O2 Zn2 N1 76.10(9) 6_566 6_566 ? O5 Zn2 N1 95.78(10) 4 6_566 ? O8 Zn2 N1 88.94(10) . 6_566 ? N2 Zn2 N1 94.15(10) 4 6_566 ? C1 O2 Zn1 112.91(19) . 6_565 ? C1 O2 Zn2 117.8(2) . 6_565 ? Zn1 O2 Zn2 112.02(10) 6_565 6_565 ? C7 O3 Zn1 123.9(2) . . ? C7 O4 Zn2 136.9(2) . . ? C8 O5 Zn2 114.9(2) . 4_545 ? C8 O6 Zn1 121.0(2) . 8_556 ? C14 O7 Zn1 133.2(2) . . ? C14 O8 Zn2 127.7(2) . . ? C6 N1 C2 118.1(3) . . ? C6 N1 Zn2 128.4(2) . 6_565 ? C2 N1 Zn2 113.3(2) . 6_565 ? C13 N2 C9 118.7(3) . . ? C13 N2 Zn2 128.3(2) . 4_545 ? C9 N2 Zn2 113.0(2) . 4_545 ? C15 N3 C19 117.0(3) . . ? C15 N3 Zn1 121.9(2) . . ? C19 N3 Zn1 120.5(2) . . ? O1 C1 O2 124.8(3) . . ? O1 C1 C2 120.4(3) . . ? O2 C1 C2 114.8(3) . . ? N1 C2 C3 122.3(3) . . ? N1 C2 C1 115.4(3) . . ? C3 C2 C1 122.3(3) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 118.1(3) . . ? C6 C5 C7 120.4(3) . . ? C4 C5 C7 121.5(3) . . ? N1 C6 C5 123.5(3) . . ? N1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? O4 C7 O3 126.9(3) . . ? O4 C7 C5 117.5(3) . . ? O3 C7 C5 115.6(3) . . ? O5 C8 O6 126.0(3) . . ? O5 C8 C9 117.5(3) . . ? O6 C8 C9 116.5(3) . . ? N2 C9 C10 122.5(3) . . ? N2 C9 C8 114.5(3) . . ? C10 C9 C8 123.0(3) . . ? C9 C10 C11 118.4(3) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 118.1(3) . . ? C11 C12 C14 123.1(3) . . ? C13 C12 C14 118.8(3) . . ? N2 C13 C12 122.5(3) . . ? N2 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? O7 C14 O8 127.5(3) . . ? O7 C14 C12 116.2(3) . . ? O8 C14 C12 116.2(3) . . ? N3 C15 C16 123.3(3) . . ? N3 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 117.0(3) . . ? C18 C17 C20 118.9(3) . . ? C16 C17 C20 124.1(3) . . ? C19 C18 C17 119.6(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? N3 C19 C18 123.5(3) . . ? N3 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? C20 C20 C17 125.6(4) 7_545 . ? C20 C20 H20 117.2 7_545 . ? C17 C20 H20 117.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.511 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.097 #End of the file