# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Wolfgang Schmitt' _publ_contact_author_email schmittw@tcd.ie _publ_section_title ; Extending the family of Zn-based MOFs: Synthetic approaches to chiral framework structures and MOFs with large pores and channels ; _publ_requested_category CM _publ_author_name 'Wolfgang Schmitt' # Attachment '- TCM-1.cif' data_Zn3MOF_j017 _database_code_depnum_ccdc_archive 'CCDC 810330' #TrackingRef '- TCM-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Zn3(BTEB)2(DMF)2) (TCM-1)' _chemical_melting_point ? _chemical_formula_moiety 'C72 H44 N2 O14 Zn3' _chemical_formula_sum 'C72 H44 N2 O14 Zn3' _chemical_formula_weight 1357.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 2 2' _symmetry_space_group_name_Hall 'P 4cw 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z+1/2' '-x, y, -z' '-y, -x, -z+3/4' 'y, x, -z+1/4' 'y, -x, z+1/4' '-y, x, z+3/4' _cell_length_a 20.269(2) _cell_length_b 20.269(2) _cell_length_c 39.645(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16287(3) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 5813 _cell_measurement_theta_min 2.2468 _cell_measurement_theta_max 18.8257 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.754197 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 APEX CCD' _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0(2) _diffrn_reflns_number 77843 _diffrn_reflns_av_R_equivalents 0.1204 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.71 _reflns_number_total 15488 _reflns_number_gt 6650 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Smart _computing_data_reduction Saintplus _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0224P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.082(9) _refine_ls_number_reflns 15488 _refine_ls_number_parameters 391 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 0.762 _refine_ls_restrained_S_all 0.762 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.936 0.000 10.1 -0.5 2 -0.001 0.517 0.104 11031.7 4104.9 3 0.000 0.064 0.500 10.1 -0.4 4 0.064 1.000 0.750 10.1 -0.4 5 0.936 0.000 0.250 10.2 -0.5 _platon_squeeze_details ; ? ; 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 0.16811(2) 0.0000 0.2500 0.07140(15) Uani 1 2 d S . . Zn2 Zn 0.168079(17) -0.145433(17) 0.299124(8) 0.08123(12) Uani 1 1 d . . . O1 O 0.16968(9) 0.01580(9) 0.30166(4) 0.0820(6) Uani 1 1 d . . . O2 O 0.15036(10) -0.07614(11) 0.33134(4) 0.0812(6) Uani 1 1 d . . . O3 O 0.14902(13) 0.73685(11) 0.46111(6) 0.1117(9) Uani 1 1 d . . . O4 O 0.07150(13) 0.76064(12) 0.50008(6) 0.1167(8) Uani 1 1 d . . . O5 O -0.10922(11) 0.17329(12) 0.76274(5) 0.1026(8) Uani 1 1 d . . . O6 O -0.09326(10) 0.06920(12) 0.75704(5) 0.0905(7) Uani 1 1 d . . . O7 O 0.16226(14) -0.22431(11) 0.32943(6) 0.1325(9) Uani 1 1 d D . . N1 N 0.1297(4) -0.3084(4) 0.3688(2) 0.344(3) Uiso 1 1 d D . . C1 C 0.15612(15) -0.01444(18) 0.32782(7) 0.0725(8) Uani 1 1 d . . . C2 C 0.14420(15) 0.02579(18) 0.35960(7) 0.0753(9) Uani 1 1 d . . . C3 C 0.14981(18) 0.0924(2) 0.35882(8) 0.0984(11) Uani 1 1 d . . . H3 H 0.1619 0.1134 0.3386 0.118 Uiso 1 1 calc R . . C4 C 0.13795(18) 0.13015(17) 0.38735(9) 0.1160(13) Uani 1 1 d . . . H4 H 0.1422 0.1763 0.3867 0.139 Uiso 1 1 calc R . . C5 C 0.11923(17) 0.0974(2) 0.41751(9) 0.0970(11) Uani 1 1 d . . . C6 C 0.11407(17) 0.0296(2) 0.41808(8) 0.1007(12) Uani 1 1 d . . . H6 H 0.1024 0.0082 0.4382 0.121 Uiso 1 1 calc R . . C7 C 0.12591(15) -0.00774(17) 0.38907(8) 0.0929(10) Uani 1 1 d . . . H7 H 0.1217 -0.0539 0.3893 0.111 Uiso 1 1 calc R . . C8 C 0.10723(19) 0.13635(18) 0.44788(10) 0.1110(12) Uani 1 1 d . . . C9 C 0.09925(19) 0.1685(2) 0.47208(10) 0.1132(13) Uani 1 1 d . . . C10 C 0.08904(18) 0.2107(2) 0.50092(10) 0.1060(11) Uani 1 1 d . . . C11 C 0.09400(18) 0.2784(2) 0.49756(9) 0.1131(12) Uani 1 1 d . . . H11 H 0.1043 0.2963 0.4763 0.136 Uiso 1 1 calc R . . C12 C 0.0843(2) 0.3204(2) 0.52445(11) 0.1118(12) Uani 1 1 d . . . C13 C 0.07166(18) 0.29220(19) 0.55730(9) 0.1057(12) Uani 1 1 d . . . H13 H 0.0659 0.3195 0.5763 0.127 Uiso 1 1 calc R . . C14 C 0.06817(18) 0.2243(2) 0.56033(9) 0.1057(12) Uani 1 1 d . . . C15 C 0.07736(18) 0.18149(18) 0.53263(10) 0.1116(12) Uani 1 1 d . . . H15 H 0.0758 0.1354 0.5352 0.134 Uiso 1 1 calc R . . C16 C 0.0906(3) 0.3848(3) 0.52107(11) 0.1397(19) Uani 1 1 d . . . C17 C 0.0925(2) 0.4440(3) 0.51690(10) 0.1400(17) Uani 1 1 d . . . C18 C 0.1010(3) 0.5167(2) 0.50869(12) 0.1288(15) Uani 1 1 d . . . C19 C 0.1371(2) 0.5375(2) 0.48198(11) 0.1425(18) Uani 1 1 d . . . H19 H 0.1598 0.5068 0.4685 0.171 Uiso 1 1 calc R . . C20 C 0.1403(2) 0.6029(2) 0.47463(9) 0.1281(14) Uani 1 1 d . . . H20 H 0.1656 0.6169 0.4561 0.154 Uiso 1 1 calc R . . C21 C 0.10756(18) 0.6490(2) 0.49374(10) 0.1008(11) Uani 1 1 d . . . C22 C 0.07170(19) 0.6283(2) 0.52198(10) 0.1072(12) Uani 1 1 d . . . H22 H 0.0516 0.6598 0.5360 0.129 Uiso 1 1 calc R . . C23 C 0.0659(2) 0.5652(3) 0.52902(10) 0.1267(14) Uani 1 1 d . . . H23 H 0.0392 0.5514 0.5471 0.152 Uiso 1 1 calc R . . C24 C 0.1105(2) 0.7223(2) 0.48359(10) 0.0990(12) Uani 1 1 d . . . C25 C 0.0518(2) 0.19707(17) 0.59345(10) 0.1132(13) Uani 1 1 d . . . C26 C 0.03613(18) 0.18147(16) 0.62054(10) 0.1055(12) Uani 1 1 d . . . C27 C 0.01127(18) 0.1654(2) 0.65428(8) 0.0991(10) Uani 1 1 d . . . C28 C -0.0176(2) 0.21630(18) 0.67163(10) 0.1347(16) Uani 1 1 d . . . H28 H -0.0175 0.2592 0.6626 0.162 Uiso 1 1 calc R . . C29 C -0.04664(19) 0.2042(2) 0.70201(10) 0.1241(13) Uani 1 1 d . . . H29 H -0.0646 0.2396 0.7143 0.149 Uiso 1 1 calc R . . C30 C -0.05026(17) 0.1426(2) 0.71496(8) 0.0888(10) Uani 1 1 d . . . C31 C -0.01694(15) 0.09076(17) 0.69755(9) 0.0832(9) Uani 1 1 d . . . H31 H -0.0152 0.0484 0.7071 0.100 Uiso 1 1 calc R . . C32 C 0.01224(17) 0.1021(2) 0.66725(9) 0.0926(10) Uani 1 1 d . . . H32 H 0.0327 0.0676 0.6553 0.111 Uiso 1 1 calc R . . C33 C -0.08670(17) 0.1262(2) 0.74735(9) 0.0903(11) Uani 1 1 d . . . C34 C 0.1205(5) -0.2529(5) 0.3468(2) 0.363(6) Uiso 1 1 d D . . H34 H 0.0773 -0.2363 0.3454 0.435 Uiso 1 1 calc R . . C35 C 0.2018(7) -0.3281(8) 0.3696(4) 0.644(11) Uiso 1 1 d D . . C36 C 0.0703(5) -0.3144(5) 0.3917(2) 0.390(5) Uiso 1 1 d 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 0.0752(4) 0.0954(4) 0.0435(3) 0.0060(3) 0.000 0.000 Zn2 0.0930(3) 0.0966(3) 0.0542(2) 0.0049(2) -0.0015(2) 0.0031(2) O1 0.0996(15) 0.1079(15) 0.0385(11) 0.0075(11) 0.0067(12) -0.0220(12) O2 0.1013(17) 0.0950(16) 0.0473(12) 0.0058(12) 0.0070(11) 0.0066(15) O3 0.151(2) 0.1029(18) 0.0814(19) 0.0100(14) 0.0211(17) 0.0151(16) O4 0.166(2) 0.112(2) 0.0719(16) -0.0027(15) 0.0062(17) 0.0518(16) O5 0.1277(19) 0.115(2) 0.0653(16) -0.0069(14) 0.0201(13) -0.0224(16) O6 0.1039(17) 0.1050(19) 0.0627(15) 0.0078(14) -0.0010(12) -0.0260(15) O7 0.167(2) 0.1254(19) 0.105(2) 0.0294(15) 0.0056(18) -0.0217(19) C1 0.073(2) 0.089(3) 0.056(2) 0.002(2) -0.0031(17) 0.003(2) C2 0.091(2) 0.087(3) 0.048(2) -0.0071(19) -0.0052(17) -0.007(2) C3 0.148(3) 0.105(3) 0.041(2) 0.002(2) 0.004(2) -0.018(3) C4 0.187(4) 0.096(3) 0.065(2) 0.010(2) -0.003(2) -0.013(3) C5 0.126(3) 0.109(3) 0.057(3) -0.013(2) 0.006(2) 0.005(2) C6 0.145(3) 0.106(3) 0.052(2) -0.002(2) 0.012(2) -0.006(3) C7 0.126(3) 0.094(3) 0.058(2) 0.006(2) 0.004(2) -0.011(2) C8 0.164(4) 0.105(3) 0.064(3) -0.003(2) -0.004(3) -0.007(2) C9 0.171(4) 0.110(3) 0.058(3) 0.000(2) 0.007(2) -0.014(3) C10 0.150(3) 0.107(3) 0.060(2) -0.012(3) 0.010(2) -0.014(3) C11 0.181(4) 0.100(3) 0.058(3) 0.005(3) 0.018(2) -0.009(3) C12 0.163(4) 0.085(3) 0.088(3) 0.005(3) 0.025(3) -0.002(3) C13 0.170(4) 0.078(3) 0.069(3) -0.017(2) 0.024(2) -0.005(3) C14 0.155(3) 0.104(3) 0.058(2) -0.004(2) 0.027(2) -0.027(3) C15 0.163(3) 0.094(3) 0.077(3) -0.003(3) 0.023(3) -0.014(2) C16 0.237(5) 0.090(4) 0.092(3) 0.012(3) 0.027(3) -0.003(4) C17 0.173(4) 0.166(5) 0.082(3) 0.007(4) 0.012(3) 0.008(5) C18 0.210(5) 0.083(4) 0.094(4) -0.005(3) -0.007(3) 0.012(3) C19 0.251(5) 0.078(3) 0.099(3) 0.015(2) 0.079(3) 0.024(3) C20 0.185(4) 0.112(4) 0.087(3) 0.002(3) 0.038(3) 0.026(3) C21 0.124(3) 0.109(4) 0.069(3) -0.001(3) 0.008(2) 0.025(3) C22 0.147(3) 0.096(3) 0.078(3) 0.010(2) 0.022(2) 0.022(3) C23 0.146(4) 0.140(4) 0.095(3) 0.032(3) 0.025(3) 0.012(4) C24 0.131(4) 0.097(4) 0.069(3) -0.005(3) -0.027(3) 0.021(3) C25 0.178(4) 0.095(3) 0.066(3) -0.011(2) 0.016(3) -0.024(2) C26 0.155(3) 0.091(3) 0.071(3) -0.001(2) 0.016(3) -0.014(2) C27 0.133(3) 0.099(3) 0.065(2) -0.009(3) 0.013(2) -0.020(3) C28 0.256(5) 0.072(3) 0.077(3) 0.007(2) 0.053(3) 0.000(3) C29 0.199(4) 0.091(3) 0.083(3) -0.007(3) 0.045(3) 0.007(3) C30 0.126(3) 0.086(3) 0.054(2) 0.003(2) 0.012(2) -0.015(3) C31 0.092(3) 0.092(3) 0.066(2) 0.006(2) 0.007(2) -0.018(2) C32 0.112(3) 0.097(3) 0.069(3) -0.002(2) 0.005(2) -0.006(2) C33 0.104(3) 0.106(4) 0.061(3) -0.025(3) 0.007(2) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 2.046(3) 8_654 ? Zn1 O4 2.046(3) 5_655 ? Zn1 O1 2.0731(17) . ? Zn1 O1 2.0731(17) 3 ? Zn1 O6 2.085(2) 4_556 ? Zn1 O6 2.085(2) 2_554 ? Zn2 O2 1.932(2) . ? Zn2 O5 1.955(2) 2_554 ? Zn2 O3 1.970(2) 5_655 ? Zn2 O7 2.004(2) . ? O1 C1 1.236(3) . ? O2 C1 1.264(3) . ? O3 C24 1.220(4) . ? O3 Zn2 1.970(2) 5_565 ? O4 C24 1.288(4) . ? O4 Zn1 2.046(3) 5_565 ? O5 C33 1.221(3) . ? O5 Zn2 1.955(2) 2 ? O6 C33 1.226(4) . ? O6 Zn1 2.085(2) 2 ? O7 C34 1.234(8) . ? N1 C34 1.436(9) . ? N1 C36 1.512(9) . ? N1 C35 1.514(12) . ? C1 C2 1.520(4) . ? C2 C3 1.356(4) . ? C2 C7 1.401(4) . ? C3 C4 1.386(4) . ? C3 H3 0.9400 . ? C4 C5 1.419(4) . ? C4 H4 0.9400 . ? C5 C6 1.380(4) . ? C5 C8 1.460(5) . ? C6 C7 1.397(4) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.171(5) . ? C9 C10 1.443(5) . ? C10 C11 1.383(4) . ? C10 C15 1.409(4) . ? C11 C12 1.378(4) . ? C11 H11 0.9400 . ? C12 C16 1.319(5) . ? C12 C13 1.445(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9400 . ? C14 C15 1.411(4) . ? C14 C25 1.462(4) . ? C15 H15 0.9400 . ? C16 C17 1.213(6) . ? C17 C18 1.517(6) . ? C18 C19 1.354(5) . ? C18 C23 1.458(5) . ? C19 C20 1.358(4) . ? C19 H19 0.9400 . ? C20 C21 1.374(4) . ? C20 H20 0.9400 . ? C21 C22 1.399(4) . ? C21 C24 1.540(5) . ? C22 C23 1.315(5) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C25 C26 1.164(4) . ? C26 C27 1.466(4) . ? C27 C28 1.371(4) . ? C27 C32 1.383(4) . ? C28 C29 1.363(4) . ? C28 H28 0.9400 . ? C29 C30 1.352(4) . ? C29 H29 0.9400 . ? C30 C31 1.426(4) . ? C30 C33 1.518(5) . ? C31 C32 1.359(4) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C34 H34 0.9400 . ? 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 O4 Zn1 O4 90.20(15) 8_654 5_655 ? O4 Zn1 O1 83.00(8) 8_654 . ? O4 Zn1 O1 95.75(8) 5_655 . ? O4 Zn1 O1 95.75(8) 8_654 3 ? O4 Zn1 O1 83.00(8) 5_655 3 ? O1 Zn1 O1 178.25(10) . 3 ? O4 Zn1 O6 92.14(10) 8_654 4_556 ? O4 Zn1 O6 171.88(9) 5_655 4_556 ? O1 Zn1 O6 92.25(8) . 4_556 ? O1 Zn1 O6 89.02(7) 3 4_556 ? O4 Zn1 O6 171.88(9) 8_654 2_554 ? O4 Zn1 O6 92.14(10) 5_655 2_554 ? O1 Zn1 O6 89.02(7) . 2_554 ? O1 Zn1 O6 92.25(8) 3 2_554 ? O6 Zn1 O6 86.61(13) 4_556 2_554 ? O2 Zn2 O5 125.75(9) . 2_554 ? O2 Zn2 O3 110.16(10) . 5_655 ? O5 Zn2 O3 115.73(10) 2_554 5_655 ? O2 Zn2 O7 99.94(9) . . ? O5 Zn2 O7 100.14(10) 2_554 . ? O3 Zn2 O7 98.72(11) 5_655 . ? C1 O1 Zn1 138.5(2) . . ? C1 O2 Zn2 128.98(19) . . ? C24 O3 Zn2 111.3(3) . 5_565 ? C24 O4 Zn1 149.4(2) . 5_565 ? C33 O5 Zn2 111.8(2) . 2 ? C33 O6 Zn1 132.2(2) . 2 ? C34 O7 Zn2 138.5(6) . . ? C34 N1 C36 108.9(7) . . ? C34 N1 C35 110.2(9) . . ? C36 N1 C35 137.2(12) . . ? O1 C1 O2 127.2(3) . . ? O1 C1 C2 117.7(3) . . ? O2 C1 C2 115.1(3) . . ? C3 C2 C7 121.6(3) . . ? C3 C2 C1 120.1(3) . . ? C7 C2 C1 118.2(3) . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 120.0(3) . . ? C6 C5 C8 120.8(4) . . ? C4 C5 C8 119.2(4) . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 118.0(3) . . ? C6 C7 H7 121.0 . . ? C2 C7 H7 121.0 . . ? C9 C8 C5 178.1(5) . . ? C8 C9 C10 177.4(4) . . ? C11 C10 C15 121.0(4) . . ? C11 C10 C9 120.1(4) . . ? C15 C10 C9 118.8(4) . . ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C16 C12 C11 121.3(4) . . ? C16 C12 C13 120.0(4) . . ? C11 C12 C13 118.6(4) . . ? C14 C13 C12 118.7(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 122.5(3) . . ? C13 C14 C25 117.7(3) . . ? C15 C14 C25 119.8(4) . . ? C10 C15 C14 117.3(3) . . ? C10 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C17 C16 C12 175.8(6) . . ? C16 C17 C18 173.4(5) . . ? C19 C18 C23 119.0(4) . . ? C19 C18 C17 122.1(4) . . ? C23 C18 C17 118.7(5) . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 121.4(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C22 119.2(4) . . ? C20 C21 C24 119.5(4) . . ? C22 C21 C24 121.2(4) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C18 119.7(4) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? O3 C24 O4 128.1(4) . . ? O3 C24 C21 116.7(4) . . ? O4 C24 C21 115.2(4) . . ? C26 C25 C14 173.2(4) . . ? C25 C26 C27 175.1(5) . . ? C28 C27 C32 121.2(3) . . ? C28 C27 C26 116.0(4) . . ? C32 C27 C26 122.7(4) . . ? C29 C28 C27 119.5(3) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C30 C29 C28 121.7(3) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 118.1(3) . . ? C29 C30 C33 123.3(4) . . ? C31 C30 C33 118.6(4) . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C27 118.7(3) . . ? C31 C32 H32 120.7 . . ? C27 C32 H32 120.7 . . ? O5 C33 O6 122.7(4) . . ? O5 C33 C30 115.8(4) . . ? O6 C33 C30 121.6(4) . . ? O7 C34 N1 128.1(9) . . ? O7 C34 H34 116.0 . . ? N1 C34 H34 116.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.390 _refine_diff_density_min -0.154 _refine_diff_density_rms 0.025 # Attachment '- TCM-2.cif' data_j016_Zn5MOF _database_code_depnum_ccdc_archive 'CCDC 843699' #TrackingRef '- TCM-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Department of Chemistry Trinity College Dublin Dublin 2 Dublin, Republic of Ireland ; _chemical_name_common ; Department of Chemistry Trinity College Dublin Dublin 2 Dublin, Republic of Ireland ; _chemical_melting_point ? _chemical_formula_moiety 'C105 H59 N2 O22 Zn5' _chemical_formula_sum 'C105 H59 N2 O22 Zn5' _chemical_formula_weight 2027.39 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' 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 'C 2/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 25.1355(17) _cell_length_b 37.055(2) _cell_length_c 20.2587(14) _cell_angle_alpha 90.00 _cell_angle_beta 124.71(2) _cell_angle_gamma 90.00 _cell_volume 15510(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9755 _cell_measurement_theta_min 2.2572 _cell_measurement_theta_max 26.6438 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4116 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.588903 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; Department of Chemistry Trinity College Dublin Dublin 2 Dublin, Republic of Ireland ; _diffrn_ambient_temperature 120(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 APEX CCD' _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0(2) _diffrn_reflns_number 36437 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14739 _reflns_number_gt 9682 _reflns_threshold_expression >2\s(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXS - 97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0939P)^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 14739 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.352 -0.070 -0.084 7673 1660 ' ' _platon_squeeze_details ; ; 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 0.900709(12) 0.716038(7) 0.240672(19) 0.03582(11) Uani 1 1 d . . . Zn2 Zn 0.997817(13) 0.680763(8) 0.41548(2) 0.04245(12) Uani 1 1 d . . . Zn3 Zn 1.0000 0.651625(12) 0.2500 0.0668(2) Uani 1 2 d S . . O10 O 0.94770(7) 0.74868(4) 0.19872(11) 0.0371(5) Uani 1 1 d . . . O1 O 0.98848(8) 0.68946(4) 0.31322(11) 0.0409(5) Uani 1 1 d . . . O7 O 0.92932(8) 0.75439(5) 0.33063(11) 0.0450(5) Uani 1 1 d . . . O11 O 0.82047(8) 0.74712(5) 0.16522(12) 0.0455(5) Uani 1 1 d . . . O5 O 0.84949(8) 0.68348(5) 0.27058(13) 0.0470(5) Uani 1 1 d . . . O2 O 0.91952(9) 0.62650(5) 0.19112(15) 0.0611(7) Uani 1 1 d . . . O6 O 1.00111(8) 0.73061(5) 0.45130(12) 0.0476(5) Uani 1 1 d . . . O3 O 0.86427(9) 0.67788(5) 0.14336(12) 0.0469(5) Uani 1 1 d . . . C48 C 0.5000 0.41925(9) 0.2500 0.0382(9) Uani 1 2 d S . . O8 O 1.07946(10) 0.65651(7) 0.48804(16) 0.0755(8) Uani 1 1 d . . . C45 C 0.5000 0.49033(9) 0.2500 0.0322(8) Uani 1 2 d S . . C1 C 0.86750(13) 0.64444(7) 0.14864(18) 0.0447(7) Uani 1 1 d . . . O4 O 0.91837(9) 0.65835(6) 0.39049(13) 0.0634(7) Uani 1 1 d . . . C51 C 0.55806(12) 0.32388(6) 0.29277(18) 0.0407(7) Uani 1 1 d . . . H51 H 0.5979 0.3111 0.3224 0.049 Uiso 1 1 calc R . . C44 C 0.55635(12) 0.50904(6) 0.27593(16) 0.0343(6) Uani 1 1 d . . . H44 H 0.5954 0.4962 0.2953 0.041 Uiso 1 1 calc R . . C15 C 0.53178(12) 0.48433(7) -0.05610(16) 0.0368(6) Uani 1 1 d . . . H15 H 0.5721 0.4720 -0.0258 0.044 Uiso 1 1 calc R . . C52 C 0.5000 0.30504(9) 0.2500 0.0358(9) Uani 1 2 d S . . C25 C 0.47718(12) 0.42806(7) -0.06701(16) 0.0397(7) Uani 1 1 d . . . C30 C 0.51818(12) 0.29312(7) 0.05805(17) 0.0408(7) Uani 1 1 d . . . C47 C 0.5000 0.45139(9) 0.2500 0.0340(8) Uani 1 2 d S . . C10 C 0.53060(12) 0.52127(7) -0.06999(15) 0.0358(6) Uani 1 1 d . . . C43 C 0.55599(12) 0.54705(7) 0.27365(17) 0.0356(6) Uani 1 1 d . . . C50 C 0.55794(12) 0.36135(7) 0.29234(17) 0.0415(7) Uani 1 1 d . . . H50 H 0.5978 0.3741 0.3212 0.050 Uiso 1 1 calc R . . C13 C 0.41529(12) 0.48344(7) -0.13281(15) 0.0359(6) Uani 1 1 d . . . H13 H 0.3759 0.4706 -0.1547 0.043 Uiso 1 1 calc R . . C9 C 0.58948(14) 0.54121(8) -0.03732(18) 0.0462(7) Uani 1 1 d . . . C11 C 0.47182(13) 0.53899(7) -0.11558(15) 0.0364(6) Uani 1 1 d . . . H11 H 0.4709 0.5641 -0.1254 0.044 Uiso 1 1 calc R . . C42 C 0.61248(14) 0.56613(7) 0.29099(19) 0.0446(7) Uani 1 1 d . . . C34 C 0.86295(12) 0.66332(8) 0.3264(2) 0.0482(8) Uani 1 1 d . . . C2 C 0.80641(13) 0.62265(7) 0.10249(19) 0.0509(8) Uani 1 1 d . . . N1 N 0.71498(11) 0.75196(8) 0.06520(16) 0.0625(8) Uani 1 1 d . . . C54 C 0.76500(12) 0.73453(8) 0.1239(2) 0.0529(9) Uani 1 1 d . . . H54 H 0.7584 0.7108 0.1355 0.064 Uiso 1 1 calc R . . C46 C 0.5000 0.56544(9) 0.2500 0.0385(9) Uani 1 2 d S . . H46 H 0.5000 0.5911 0.2500 0.046 Uiso 1 2 calc SR . . C27 C 0.49440(13) 0.36188(7) -0.01059(18) 0.0461(8) Uani 1 1 d . . . C31 C 0.55085(17) 0.32306(7) 0.1063(2) 0.0591(10) Uani 1 1 d . . . H31 H 0.5811 0.3201 0.1625 0.071 Uiso 1 1 calc R . . C49 C 0.5000 0.38030(9) 0.2500 0.0359(9) Uani 1 2 d S . . C12 C 0.41414(12) 0.52038(7) -0.14717(16) 0.0362(6) Uani 1 1 d . . . C14 C 0.47462(12) 0.46531(7) -0.08613(15) 0.0351(6) Uani 1 1 d . . . C16 C 0.35421(14) 0.53982(8) -0.19773(19) 0.0508(8) Uani 1 1 d . . . C41 C 0.65702(14) 0.58247(8) 0.3007(2) 0.0499(8) Uani 1 1 d . . . C38 C 0.70937(14) 0.60260(8) 0.3077(2) 0.0508(8) Uani 1 1 d . . . C8 C 0.63675(14) 0.55928(8) -0.0093(2) 0.0540(9) Uani 1 1 d . . . C29 C 0.47539(15) 0.29797(8) -0.0231(2) 0.0588(9) Uani 1 1 d . . . H29 H 0.4535 0.2777 -0.0567 0.071 Uiso 1 1 calc R . . C4 C 0.69133(14) 0.61776(8) 0.0170(2) 0.0556(9) Uani 1 1 d . . . H4 H 0.6506 0.6294 -0.0162 0.067 Uiso 1 1 calc R . . C32 C 0.53941(17) 0.35691(8) 0.0725(2) 0.0635(10) Uani 1 1 d . . . H32 H 0.5622 0.3771 0.1057 0.076 Uiso 1 1 calc R . . C3 C 0.74734(13) 0.63798(8) 0.0547(2) 0.0564(9) Uani 1 1 d . . . H3 H 0.7443 0.6634 0.0469 0.068 Uiso 1 1 calc R . . C37 C 0.70013(14) 0.61898(9) 0.2409(2) 0.0634(10) Uani 1 1 d . . . H37 H 0.6600 0.6165 0.1902 0.076 Uiso 1 1 calc R . . C35 C 0.80874(13) 0.64200(8) 0.31962(19) 0.0491(8) Uani 1 1 d . . . C26 C 0.48403(13) 0.39725(7) -0.04410(18) 0.0455(7) Uani 1 1 d . . . C5 C 0.69389(14) 0.58097(8) 0.0270(2) 0.0591(9) Uani 1 1 d . . . C20 C 0.18819(17) 0.61565(10) -0.4119(2) 0.0708(11) Uani 1 1 d . . . H20 H 0.1815 0.6252 -0.4596 0.085 Uiso 1 1 calc R . . C21 C 0.14534(17) 0.62302(10) -0.3942(3) 0.0728(11) Uani 1 1 d . . . C28 C 0.46375(15) 0.33214(8) -0.05673(19) 0.0579(9) Uani 1 1 d . . . H28 H 0.4338 0.3349 -0.1131 0.070 Uiso 1 1 calc R . . C18 C 0.25211(16) 0.57990(10) -0.2934(2) 0.0716(11) Uani 1 1 d . . . C36 C 0.74978(14) 0.63930(9) 0.2479(2) 0.0658(11) Uani 1 1 d . . . H36 H 0.7425 0.6514 0.2021 0.079 Uiso 1 1 calc R . . C40 C 0.81811(16) 0.62447(11) 0.3857(2) 0.0774(13) Uani 1 1 d . . . H40 H 0.8592 0.6257 0.4356 0.093 Uiso 1 1 calc R . . C56 C 0.7201(2) 0.78753(11) 0.0427(3) 0.0892(14) Uani 1 1 d . . . H56A H 0.7041 0.8049 0.0640 0.134 Uiso 1 1 calc R . . H56B H 0.6941 0.7894 -0.0160 0.134 Uiso 1 1 calc R . . H56C H 0.7654 0.7928 0.0646 0.134 Uiso 1 1 calc R . . C7 C 0.80943(17) 0.58598(10) 0.1121(4) 0.141(3) Uani 1 1 d . . . H7 H 0.8503 0.5747 0.1470 0.169 Uiso 1 1 calc R . . C19 C 0.24241(17) 0.59416(10) -0.3613(2) 0.0711(11) Uani 1 1 d . . . H19 H 0.2726 0.5895 -0.3743 0.085 Uiso 1 1 calc R . . C39 C 0.76912(17) 0.60522(11) 0.3806(2) 0.0790(13) Uani 1 1 d . . . H39 H 0.7762 0.5938 0.4270 0.095 Uiso 1 1 calc R . . C17 C 0.30845(15) 0.55768(9) -0.2402(2) 0.0624(10) Uani 1 1 d . . . C22 C 0.1546(2) 0.60929(13) -0.3253(3) 0.1004(16) Uani 1 1 d . . . H22 H 0.1242 0.6145 -0.3129 0.120 Uiso 1 1 calc R . . O9 O 1.04825(15) 0.65340(11) 0.5687(2) 0.1242(13) Uani 1 1 d . . . C23 C 0.2079(2) 0.58789(15) -0.2741(3) 0.1068(18) Uani 1 1 d . . . H23 H 0.2145 0.5787 -0.2262 0.128 Uiso 1 1 calc R . . C6 C 0.75466(18) 0.56539(10) 0.0722(4) 0.162(3) Uani 1 1 d . . . H6 H 0.7584 0.5398 0.0755 0.195 Uiso 1 1 calc R . . C55 C 0.65023(16) 0.73427(15) 0.0191(3) 0.1071(18) Uani 1 1 d . . . H55A H 0.6529 0.7111 0.0439 0.161 Uiso 1 1 calc R . . H55B H 0.6364 0.7303 -0.0364 0.161 Uiso 1 1 calc R . . H55C H 0.6188 0.7498 0.0193 0.161 Uiso 1 1 calc R . . C53 C 1.0000 0.76462(9) 0.2500 0.0304(8) Uiso 1 2 d S . . C24 C 0.96943(13) 0.75672(7) 0.40420(17) 0.0376(6) Uiso 1 1 d . . . C33 C 1.0859(2) 0.64637(11) 0.5496(3) 0.0744(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01627(14) 0.01859(15) 0.0482(2) 0.00427(12) 0.00386(13) -0.00025(10) Zn2 0.01912(15) 0.02342(16) 0.0557(2) 0.00810(14) 0.00403(14) -0.00053(11) Zn3 0.0243(2) 0.0239(2) 0.1109(5) 0.000 0.0141(3) 0.000 O10 0.0182(8) 0.0203(8) 0.0503(11) 0.0007(8) 0.0061(8) -0.0028(7) O1 0.0198(8) 0.0211(9) 0.0574(12) 0.0055(8) 0.0075(8) 0.0009(7) O7 0.0325(10) 0.0262(9) 0.0509(12) -0.0023(8) 0.0087(9) 0.0013(7) O11 0.0210(9) 0.0293(10) 0.0605(12) 0.0093(9) 0.0080(9) 0.0041(7) O5 0.0235(9) 0.0374(11) 0.0601(13) 0.0146(10) 0.0120(9) -0.0029(8) O2 0.0284(10) 0.0217(10) 0.0963(17) -0.0093(10) 0.0136(11) -0.0043(8) O6 0.0342(10) 0.0235(9) 0.0577(13) 0.0044(9) 0.0100(9) 0.0009(8) O3 0.0307(10) 0.0249(10) 0.0561(13) 0.0046(8) 0.0076(9) -0.0045(7) C48 0.039(2) 0.0233(19) 0.051(2) 0.000 0.0245(19) 0.000 O8 0.0359(12) 0.0689(16) 0.0847(18) 0.0333(14) 0.0125(12) 0.0087(11) C45 0.0371(19) 0.0200(17) 0.038(2) 0.000 0.0203(17) 0.000 C1 0.0302(14) 0.0318(15) 0.0559(18) -0.0074(13) 0.0150(13) -0.0083(12) O4 0.0242(10) 0.0575(13) 0.0675(14) 0.0231(11) 0.0017(10) -0.0161(9) C51 0.0212(12) 0.0231(13) 0.0586(18) -0.0010(12) 0.0114(13) 0.0005(10) C44 0.0330(13) 0.0250(13) 0.0447(16) 0.0003(11) 0.0220(12) 0.0028(10) C15 0.0243(12) 0.0359(14) 0.0342(14) -0.0006(11) 0.0072(11) 0.0025(10) C52 0.0264(17) 0.0193(17) 0.049(2) 0.000 0.0138(17) 0.000 C25 0.0297(13) 0.0345(15) 0.0407(15) -0.0014(12) 0.0116(12) 0.0016(11) C30 0.0269(13) 0.0289(14) 0.0487(17) -0.0012(12) 0.0108(13) 0.0036(10) C47 0.039(2) 0.0245(19) 0.042(2) 0.000 0.0257(18) 0.000 C10 0.0283(13) 0.0356(14) 0.0300(14) -0.0031(11) 0.0087(11) -0.0033(11) C43 0.0334(13) 0.0265(13) 0.0476(16) -0.0037(12) 0.0235(13) -0.0062(10) C50 0.0271(13) 0.0262(13) 0.0562(18) -0.0041(12) 0.0148(13) -0.0065(10) C13 0.0270(13) 0.0373(15) 0.0328(14) -0.0004(11) 0.0108(11) -0.0036(11) C9 0.0393(16) 0.0370(15) 0.0463(17) -0.0035(13) 0.0148(14) -0.0047(13) C11 0.0409(15) 0.0282(13) 0.0330(14) 0.0020(11) 0.0169(12) 0.0010(11) C42 0.0415(15) 0.0257(14) 0.0616(19) -0.0013(13) 0.0264(14) -0.0013(12) C34 0.0245(13) 0.0367(16) 0.064(2) 0.0063(15) 0.0142(14) -0.0057(11) C2 0.0332(15) 0.0306(15) 0.065(2) -0.0103(14) 0.0142(14) -0.0071(12) N1 0.0215(12) 0.079(2) 0.0565(17) 0.0130(15) 0.0042(12) 0.0165(12) C54 0.0230(13) 0.0459(17) 0.064(2) 0.0103(15) 0.0097(14) 0.0057(12) C46 0.044(2) 0.0152(16) 0.055(2) 0.000 0.0276(19) 0.000 C27 0.0398(15) 0.0283(14) 0.0532(18) 0.0041(13) 0.0163(14) 0.0067(12) C31 0.065(2) 0.0293(15) 0.0527(19) 0.0049(14) 0.0157(17) 0.0012(14) C49 0.042(2) 0.0178(17) 0.048(2) 0.000 0.0252(18) 0.000 C12 0.0319(13) 0.0334(14) 0.0347(14) 0.0060(11) 0.0138(12) 0.0085(11) C14 0.0316(13) 0.0272(13) 0.0323(14) -0.0009(11) 0.0098(11) 0.0012(10) C16 0.0389(16) 0.0462(17) 0.0516(18) 0.0134(15) 0.0164(14) 0.0098(13) C41 0.0393(16) 0.0335(15) 0.067(2) -0.0024(14) 0.0243(15) -0.0068(13) C38 0.0377(16) 0.0364(16) 0.069(2) -0.0015(15) 0.0250(15) -0.0119(12) C8 0.0391(16) 0.0388(16) 0.065(2) -0.0059(15) 0.0184(15) -0.0105(13) C29 0.0487(18) 0.0347(16) 0.055(2) -0.0026(14) 0.0065(15) -0.0029(13) C4 0.0344(15) 0.0451(18) 0.062(2) 0.0019(15) 0.0127(15) -0.0034(13) C32 0.074(2) 0.0249(15) 0.062(2) -0.0061(14) 0.0204(18) -0.0026(14) C3 0.0346(15) 0.0324(15) 0.069(2) -0.0021(14) 0.0093(15) -0.0089(12) C37 0.0311(15) 0.057(2) 0.073(2) 0.0156(18) 0.0120(16) -0.0090(14) C35 0.0285(14) 0.0358(15) 0.0596(19) 0.0085(14) 0.0112(14) -0.0104(11) C26 0.0369(15) 0.0336(16) 0.0504(18) 0.0022(13) 0.0157(14) 0.0038(12) C5 0.0355(16) 0.0433(18) 0.069(2) -0.0124(16) 0.0124(16) -0.0139(13) C20 0.056(2) 0.064(2) 0.076(3) 0.034(2) 0.028(2) 0.0195(18) C21 0.048(2) 0.063(2) 0.086(3) 0.027(2) 0.026(2) 0.0208(17) C28 0.0524(18) 0.0391(17) 0.0485(19) 0.0039(14) 0.0087(15) 0.0029(14) C18 0.0415(18) 0.070(2) 0.080(3) 0.036(2) 0.0204(18) 0.0192(16) C36 0.0310(15) 0.064(2) 0.071(2) 0.0226(18) 0.0106(16) -0.0106(14) C40 0.0427(18) 0.081(3) 0.073(2) 0.020(2) 0.0117(18) -0.0232(18) C56 0.074(3) 0.084(3) 0.093(3) 0.049(2) 0.038(2) 0.049(2) C7 0.0324(18) 0.0320(19) 0.242(6) -0.014(3) 0.009(3) -0.0052(15) C19 0.051(2) 0.076(3) 0.072(2) 0.029(2) 0.0271(19) 0.0221(18) C39 0.050(2) 0.087(3) 0.069(2) 0.019(2) 0.0159(18) -0.0264(19) C17 0.0444(18) 0.055(2) 0.071(2) 0.0207(18) 0.0233(17) 0.0148(15) C22 0.072(3) 0.122(4) 0.107(4) 0.052(3) 0.050(3) 0.057(3) O9 0.074(2) 0.165(3) 0.125(3) 0.054(2) 0.051(2) 0.070(2) C23 0.075(3) 0.146(4) 0.105(4) 0.066(3) 0.056(3) 0.059(3) C6 0.042(2) 0.032(2) 0.289(8) -0.013(3) 0.020(3) -0.0101(17) C55 0.0254(17) 0.140(4) 0.093(3) -0.010(3) -0.004(2) 0.005(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O11 2.0543(17) . ? Zn1 O1 2.0746(17) . ? Zn1 O7 2.0893(19) . ? Zn1 O5 2.090(2) . ? Zn1 O3 2.161(2) . ? Zn1 O10 2.1733(19) . ? Zn2 O8 1.935(2) . ? Zn2 O4 1.9448(19) . ? Zn2 O6 1.9689(19) . ? Zn2 O1 1.974(2) . ? Zn3 O2 1.9062(18) 2_755 ? Zn3 O2 1.9062(18) . ? Zn3 O1 2.028(2) . ? Zn3 O1 2.028(2) 2_755 ? O10 C53 1.265(2) . ? O7 C24 1.239(3) . ? O11 C54 1.238(3) . ? O5 C34 1.231(4) . ? O2 C1 1.269(3) . ? O6 C24 1.271(3) . ? O3 C1 1.242(3) . ? C48 C47 1.191(5) . ? C48 C49 1.443(5) . ? O8 C33 1.223(5) . ? C45 C44 1.384(3) . ? C45 C44 1.384(3) 2_655 ? C45 C47 1.443(5) . ? C1 C2 1.500(4) . ? O4 C34 1.265(3) . ? C51 C50 1.388(3) . ? C51 C52 1.389(3) . ? C51 H51 0.9500 . ? C44 C43 1.409(3) . ? C44 H44 0.9500 . ? C15 C14 1.391(4) . ? C15 C10 1.394(4) . ? C15 H15 0.9500 . ? C52 C51 1.389(3) 2_655 ? C52 C53 1.498(5) 3_445 ? C25 C26 1.207(4) . ? C25 C14 1.425(4) . ? C30 C29 1.371(4) . ? C30 C31 1.395(4) . ? C30 C24 1.493(4) 4_645 ? C10 C11 1.383(4) . ? C10 C9 1.435(4) . ? C43 C46 1.381(3) . ? C43 C42 1.439(4) . ? C50 C49 1.388(3) . ? C50 H50 0.9500 . ? C13 C12 1.396(4) . ? C13 C14 1.401(3) . ? C13 H13 0.9500 . ? C9 C8 1.189(4) . ? C11 C12 1.389(4) . ? C11 H11 0.9500 . ? C42 C41 1.187(4) . ? C34 C35 1.512(4) . ? C2 C3 1.352(4) . ? C2 C7 1.368(5) . ? N1 C54 1.307(4) . ? N1 C56 1.424(5) . ? N1 C55 1.490(5) . ? C54 H54 0.9500 . ? C46 C43 1.381(3) 2_655 ? C46 H46 0.9500 . ? C27 C28 1.364(4) . ? C27 C32 1.407(4) . ? C27 C26 1.430(4) . ? C31 C32 1.378(4) . ? C31 H31 0.9500 . ? C49 C50 1.388(3) 2_655 ? C12 C16 1.442(4) . ? C16 C17 1.172(4) . ? C41 C38 1.448(4) . ? C38 C37 1.376(5) . ? C38 C39 1.386(4) . ? C8 C5 1.431(4) . ? C29 C28 1.388(4) . ? C29 H29 0.9500 . ? C4 C5 1.374(4) . ? C4 C3 1.379(4) . ? C4 H4 0.9500 . ? C32 H32 0.9500 . ? C3 H3 0.9500 . ? C37 C36 1.395(4) . ? C37 H37 0.9500 . ? C35 C36 1.366(4) . ? C35 C40 1.381(5) . ? C5 C6 1.383(5) . ? C20 C21 1.342(5) . ? C20 C19 1.397(4) . ? C20 H20 0.9500 . ? C21 C22 1.375(6) . ? C21 C33 1.530(5) 1_454 ? C28 H28 0.9500 . ? C18 C19 1.359(5) . ? C18 C23 1.404(6) . ? C18 C17 1.451(4) . ? C36 H36 0.9500 . ? C40 C39 1.376(5) . ? C40 H40 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C7 C6 1.365(5) . ? C7 H7 0.9500 . ? C19 H19 0.9500 . ? C39 H39 0.9500 . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? O9 C33 1.236(5) . ? C23 H23 0.9500 . ? C6 H6 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C53 O10 1.265(2) 2_755 ? C53 C52 1.498(5) 3 ? C24 C30 1.493(4) 4_655 ? C33 C21 1.530(5) 1_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Zn1 O1 172.17(8) . . ? O11 Zn1 O7 88.40(8) . . ? O1 Zn1 O7 90.34(7) . . ? O11 Zn1 O5 91.92(8) . . ? O1 Zn1 O5 95.89(7) . . ? O7 Zn1 O5 95.89(9) . . ? O11 Zn1 O3 87.80(8) . . ? O1 Zn1 O3 93.61(7) . . ? O7 Zn1 O3 175.96(7) . . ? O5 Zn1 O3 82.86(8) . . ? O11 Zn1 O10 85.35(7) . . ? O1 Zn1 O10 86.89(7) . . ? O7 Zn1 O10 88.22(8) . . ? O5 Zn1 O10 175.01(7) . . ? O3 Zn1 O10 92.85(7) . . ? O8 Zn2 O4 119.14(10) . . ? O8 Zn2 O6 110.61(10) . . ? O4 Zn2 O6 108.54(10) . . ? O8 Zn2 O1 108.30(11) . . ? O4 Zn2 O1 107.80(9) . . ? O6 Zn2 O1 100.87(8) . . ? O2 Zn3 O2 121.52(11) 2_755 . ? O2 Zn3 O1 115.14(9) 2_755 . ? O2 Zn3 O1 104.51(8) . . ? O2 Zn3 O1 104.51(8) 2_755 2_755 ? O2 Zn3 O1 115.14(9) . 2_755 ? O1 Zn3 O1 92.53(11) . 2_755 ? C53 O10 Zn1 118.73(14) . . ? Zn2 O1 Zn3 125.14(8) . . ? Zn2 O1 Zn1 105.31(9) . . ? Zn3 O1 Zn1 110.94(9) . . ? C24 O7 Zn1 137.49(18) . . ? C54 O11 Zn1 122.83(18) . . ? C34 O5 Zn1 136.40(17) . . ? C1 O2 Zn3 119.00(16) . . ? C24 O6 Zn2 124.10(18) . . ? C1 O3 Zn1 127.0(2) . . ? C47 C48 C49 180.000(1) . . ? C33 O8 Zn2 112.6(3) . . ? C44 C45 C44 119.9(3) . 2_655 ? C44 C45 C47 120.07(15) . . ? C44 C45 C47 120.07(15) 2_655 . ? O3 C1 O2 124.9(2) . . ? O3 C1 C2 119.3(2) . . ? O2 C1 C2 115.7(2) . . ? C34 O4 Zn2 124.9(2) . . ? C50 C51 C52 120.1(2) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C45 C44 C43 120.2(2) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C14 C15 C10 120.7(2) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C51 C52 C51 119.6(3) . 2_655 ? C51 C52 C53 120.19(15) . 3_445 ? C51 C52 C53 120.19(15) 2_655 3_445 ? C26 C25 C14 174.2(3) . . ? C29 C30 C31 118.9(3) . . ? C29 C30 C24 121.7(2) . 4_645 ? C31 C30 C24 119.5(3) . 4_645 ? C48 C47 C45 180.000(1) . . ? C11 C10 C15 119.5(2) . . ? C11 C10 C9 119.5(2) . . ? C15 C10 C9 121.0(2) . . ? C46 C43 C44 119.4(2) . . ? C46 C43 C42 120.8(2) . . ? C44 C43 C42 119.7(2) . . ? C49 C50 C51 120.5(2) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C8 C9 C10 176.3(3) . . ? C10 C11 C12 120.6(2) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C41 C42 C43 176.1(4) . . ? O5 C34 O4 126.6(3) . . ? O5 C34 C35 118.1(2) . . ? O4 C34 C35 115.2(3) . . ? C3 C2 C7 117.9(3) . . ? C3 C2 C1 122.5(2) . . ? C7 C2 C1 119.5(3) . . ? C54 N1 C56 122.2(3) . . ? C54 N1 C55 119.6(3) . . ? C56 N1 C55 118.1(3) . . ? O11 C54 N1 123.9(3) . . ? O11 C54 H54 118.0 . . ? N1 C54 H54 118.0 . . ? C43 C46 C43 120.9(3) 2_655 . ? C43 C46 H46 119.6 2_655 . ? C43 C46 H46 119.6 . . ? C28 C27 C32 118.0(3) . . ? C28 C27 C26 122.4(3) . . ? C32 C27 C26 119.6(3) . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C50 C49 C50 119.2(3) . 2_655 ? C50 C49 C48 120.39(15) . . ? C50 C49 C48 120.39(15) 2_655 . ? C11 C12 C13 119.9(2) . . ? C11 C12 C16 118.2(2) . . ? C13 C12 C16 121.8(2) . . ? C15 C14 C13 119.3(2) . . ? C15 C14 C25 119.8(2) . . ? C13 C14 C25 120.9(2) . . ? C17 C16 C12 174.1(4) . . ? C42 C41 C38 176.8(4) . . ? C37 C38 C39 119.4(3) . . ? C37 C38 C41 119.7(3) . . ? C39 C38 C41 120.9(3) . . ? C9 C8 C5 178.0(4) . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C31 C32 C27 120.8(3) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? C2 C3 C4 121.8(3) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C38 C37 C36 119.9(3) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C36 C35 C40 118.7(3) . . ? C36 C35 C34 120.7(3) . . ? C40 C35 C34 120.6(3) . . ? C25 C26 C27 175.4(3) . . ? C4 C5 C6 116.9(3) . . ? C4 C5 C8 122.2(3) . . ? C6 C5 C8 120.9(3) . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.9(3) . . ? C20 C21 C33 120.6(4) . 1_454 ? C22 C21 C33 119.5(4) . 1_454 ? C27 C28 C29 121.5(3) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C19 C18 C23 119.1(3) . . ? C19 C18 C17 120.5(4) . . ? C23 C18 C17 120.4(4) . . ? C35 C36 C37 120.9(3) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C39 C40 C35 121.4(3) . . ? C39 C40 H40 119.3 . . ? C35 C40 H40 119.3 . . ? N1 C56 H56A 109.5 . . ? N1 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N1 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C6 C7 C2 121.0(3) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C16 C17 C18 179.3(4) . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 119.5(4) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? N1 C55 H55A 109.5 . . ? N1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O10 C53 O10 124.3(3) 2_755 . ? O10 C53 C52 117.83(15) 2_755 3 ? O10 C53 C52 117.83(15) . 3 ? O7 C24 O6 125.7(3) . . ? O7 C24 C30 118.0(2) . 4_655 ? O6 C24 C30 116.4(2) . 4_655 ? O8 C33 O9 125.1(4) . . ? O8 C33 C21 115.9(4) . 1_656 ? O9 C33 C21 119.0(4) . 1_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.312 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.075