# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(Zn(bpdc-[NO2]2(dabco)(DMF))n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Zn(bpdc-[NO2]2(dabco)(DMF))n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H10 N4 O9 Zn' _chemical_formula_weight 515.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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 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 13.7580(11) _cell_length_b 25.2156(18) _cell_length_c 14.9205(11) _cell_angle_alpha 90.00 _cell_angle_beta 111.399(4) _cell_angle_gamma 90.00 _cell_volume 4819.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 4471 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 50.14 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.826 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _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 8945 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 50.31 _reflns_number_total 2463 _reflns_number_gt 2156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. High UEq for N5 and C100 are due to the disordered of DMF molecules. High ADP for C101A and 101B are due to the severely disordered DMF molecules. No hydrogen atom is added to the DMF due to the disorders. We have tried our best to resolve this disordered. The low value of calculated sin(theta_max)/wavelengh is due to the quality of the structure. SQUEEZE is also applied to remove any unresolved electron density belong to the disorders as well as solvents. The ratio max/min residual electron density is little high potentially due to the unresolved disorders. ; 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 0.000 0.889 0.250 35 2 ' ' 2 0.000 0.982 0.250 6 1 ' ' 3 0.000 0.111 0.750 36 2 ' ' 4 0.000 0.018 0.750 5 1 ' ' 5 0.250 0.250 0.500 140 38 ' ' 6 0.250 0.750 1.000 140 38 ' ' 7 0.500 0.389 0.250 35 2 ' ' 8 0.500 0.611 0.750 36 2 ' ' 9 0.500 0.482 0.250 6 1 ' ' 10 0.500 0.518 0.750 5 1 ' ' 11 0.750 0.750 0.500 140 38 ' ' 12 0.750 0.250 1.000 140 38 ' ' _platon_squeeze_details ? _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^)+(0.1218P)^2^+14.7045P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2463 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1942 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 N1 N 0.4214(4) 0.01529(15) 0.1693(3) 0.0556(13) Uani 1 1 d . . . O1 O 0.3761(4) 0.07082(18) -0.0408(4) 0.0887(14) Uani 1 1 d . . . O2 O 0.2426(4) 0.08881(16) 0.0020(3) 0.0778(12) Uani 1 1 d . . . C9 C 0.3239(7) -0.1871(3) -0.1836(5) 0.085(2) Uani 1 1 d . . . C4 C 0.3601(6) 0.1695(3) -0.1307(5) 0.0785(19) Uani 1 1 d . . . H4 H 0.4134 0.1467 -0.1302 0.094 Uiso 1 1 calc R . . C5 C 0.3503(6) 0.2180(3) -0.1758(5) 0.084(2) Uani 1 1 d . . . C1 C 0.3059(6) 0.1002(3) -0.0391(5) 0.0697(17) Uani 1 1 d . . . C8 C 0.2604(7) 0.3043(3) -0.2332(5) 0.086(2) Uani 1 1 d . . . C2 C 0.2156(5) 0.1888(3) -0.0879(4) 0.0679(17) Uani 1 1 d . . . H2 H 0.1701 0.1795 -0.0573 0.081 Uiso 1 1 calc R . . C10 C 0.3258(7) -0.1406(3) -0.1301(5) 0.091(2) Uani 1 1 d . . . H10 H 0.3819 -0.1348 -0.0728 0.109 Uiso 1 1 calc R . . C3 C 0.2934(5) 0.1544(2) -0.0868(4) 0.0598(15) Uani 1 1 d . . . C6 C 0.2044(6) 0.2378(3) -0.1349(5) 0.080(2) Uani 1 1 d . . . C7 C 0.2726(6) 0.2536(3) -0.1796(4) 0.0755(19) Uani 1 1 d . . . O7 O 0.3222(6) -0.0529(2) -0.0209(5) 0.1139(19) Uani 1 1 d . . . O8 O 0.1832(6) -0.0201(3) -0.1306(6) 0.130(2) Uani 1 1 d . . . C13 C 0.2478(6) -0.1039(3) -0.1602(6) 0.082(2) Uani 1 1 d . . . C11 C 0.1613(7) -0.1561(3) -0.2956(6) 0.093(2) Uani 1 1 d . . . C12 C 0.1656(7) -0.1112(3) -0.2433(6) 0.103(2) Uani 1 1 d . . . H12 H 0.1127 -0.0860 -0.2645 0.123 Uiso 1 1 calc R . . C14 C 0.2522(8) -0.0539(4) -0.0986(7) 0.098(2) Uani 1 1 d . . . C15 C 0.3988(9) -0.0140(4) 0.2496(8) 0.077(3) Uani 0.632(5) 1 d P . 2 H15A H 0.3365 0.0005 0.2563 0.092 Uiso 0.632(5) 1 calc PR . 2 H15B H 0.3866 -0.0513 0.2333 0.092 Uiso 0.632(5) 1 calc PR . 2 C17 C 0.5097(9) -0.0082(5) 0.1568(8) 0.084(4) Uani 0.632(5) 1 d P . 2 H17A H 0.5304 0.0136 0.1131 0.101 Uiso 0.632(5) 1 calc PR . 2 H17B H 0.4904 -0.0428 0.1275 0.101 Uiso 0.632(5) 1 calc PR . 2 C19 C 0.4484(9) 0.0700(4) 0.2070(8) 0.075(3) Uani 0.632(5) 1 d P . 2 H19A H 0.3934 0.0840 0.2265 0.090 Uiso 0.632(5) 1 calc PR . 2 H19B H 0.4543 0.0927 0.1568 0.090 Uiso 0.632(5) 1 calc PR . 2 N2A N -0.0656(9) -0.1539(4) -0.1143(8) 0.093(3) Uani 0.632(5) 1 d P . 2 N3A N 0.1090(9) 0.2668(4) -0.1301(7) 0.089(3) Uani 0.632(5) 1 d P . 2 O3A O 0.0409(11) 0.2457(5) -0.1131(15) 0.197(8) Uani 0.632(5) 1 d P . 2 O4A O 0.1081(7) 0.3134(3) -0.1460(5) 0.097(3) Uani 0.632(5) 1 d P . 2 O5A O -0.0643(6) -0.1851(3) -0.0520(5) 0.089(2) Uani 0.632(5) 1 d P . 2 O6A O 0.0115(8) -0.1244(4) -0.1033(7) 0.125(4) Uani 0.632(5) 1 d P . 2 102A C 0.015(2) -0.0241(11) 0.1461(15) 0.188(10) Uani 0.632(5) 1 d P . 2 101A C 0.026(4) -0.1077(17) 0.120(3) 0.45(4) Uani 0.632(5) 1 d P . 2 C16 C 0.4605(13) -0.0408(5) 0.2013(11) 0.056(4) Uani 0.368(5) 1 d P . 1 H16A H 0.4023 -0.0630 0.1996 0.067 Uiso 0.368(5) 1 calc PR . 1 H16B H 0.4902 -0.0556 0.1570 0.067 Uiso 0.368(5) 1 calc PR . 1 C18 C 0.5161(12) 0.0442(6) 0.1625(11) 0.057(4) Uani 0.368(5) 1 d P . 1 H18A H 0.4986 0.0810 0.1457 0.069 Uiso 0.368(5) 1 calc PR . 1 H18B H 0.5359 0.0281 0.1126 0.069 Uiso 0.368(5) 1 calc PR . 1 C20 C 0.3918(12) 0.0408(6) 0.2398(11) 0.054(4) Uani 0.368(5) 1 d P . 1 H20A H 0.3348 0.0214 0.2481 0.064 Uiso 0.368(5) 1 calc PR . 1 H20B H 0.3672 0.0763 0.2181 0.064 Uiso 0.368(5) 1 calc PR . 1 N2B N -0.0657(13) 0.2836(7) -0.1461(10) 0.082(5) Uani 0.368(5) 1 d P . 1 N3B N 0.4340(18) -0.2178(8) 0.2771(15) 0.119(7) Uani 0.368(5) 1 d P . 1 O3B O 0.5000 -0.1737(7) 0.2500 0.36(2) Uani 0.736(10) 2 d SP . 1 O4B O 0.4682(13) -0.2608(6) 0.2636(13) 0.119(6) Uani 0.368(5) 1 d P . 1 O5B O -0.0657(14) 0.2367(6) -0.1639(10) 0.103(5) Uani 0.368(5) 1 d P . 1 O6B O 0.0207(12) 0.3057(7) -0.0988(11) 0.119(6) Uani 0.368(5) 1 d P . 1 102B C -0.004(7) -0.093(3) 0.005(10) 0.69(16) Uani 0.368(5) 1 d P . 1 101B C 0.118(3) -0.102(3) 0.190(4) 0.36(5) Uani 0.368(5) 1 d P . 1 O9 O 0.1861(6) -0.0095(2) 0.0894(5) 0.119(2) Uani 1 1 d . . . N5 N 0.0852(6) -0.0680(4) 0.1245(6) 0.123(3) Uani 1 1 d . . . C100 C 0.1403(12) -0.0428(8) 0.0859(10) 0.188(7) Uani 1 1 d . . . Zn1 Zn 0.29612(7) 0.01403(3) 0.03865(6) 0.0703(5) 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 N1 0.079(3) 0.032(3) 0.064(3) 0.000(2) 0.037(3) -0.002(2) O1 0.108(4) 0.061(3) 0.100(3) 0.010(2) 0.042(3) 0.030(3) O2 0.085(3) 0.058(3) 0.089(3) 0.000(2) 0.030(3) 0.001(2) C9 0.124(6) 0.081(5) 0.052(4) -0.011(4) 0.032(4) -0.006(4) C4 0.086(5) 0.072(5) 0.078(4) 0.006(4) 0.030(4) 0.017(4) C5 0.106(6) 0.075(5) 0.079(4) 0.008(4) 0.042(4) 0.001(4) C1 0.073(5) 0.060(4) 0.070(4) -0.014(3) 0.019(4) -0.003(4) C8 0.141(7) 0.058(4) 0.072(5) 0.011(4) 0.053(5) 0.021(5) C2 0.072(4) 0.068(4) 0.063(4) -0.001(3) 0.024(3) 0.003(3) C10 0.112(6) 0.089(6) 0.067(4) -0.007(4) 0.028(4) -0.033(5) C3 0.070(4) 0.042(3) 0.064(4) -0.001(3) 0.021(3) 0.007(3) C6 0.099(5) 0.059(4) 0.068(4) -0.001(3) 0.014(4) 0.034(4) C7 0.117(5) 0.060(4) 0.057(4) 0.008(3) 0.040(4) 0.008(4) O7 0.142(5) 0.093(4) 0.100(4) -0.025(3) 0.037(4) -0.025(4) O8 0.149(6) 0.093(5) 0.138(5) -0.022(4) 0.042(5) 0.012(4) C13 0.100(6) 0.060(4) 0.093(5) -0.016(4) 0.042(5) -0.002(4) C11 0.123(7) 0.078(5) 0.085(5) -0.020(4) 0.046(5) -0.022(5) C12 0.119(7) 0.094(6) 0.101(6) -0.024(5) 0.046(6) -0.017(5) C14 0.100(6) 0.096(7) 0.095(6) 0.009(5) 0.031(5) -0.011(5) C15 0.079(8) 0.078(8) 0.078(7) 0.000(5) 0.036(7) -0.023(6) C17 0.092(9) 0.083(9) 0.080(8) -0.010(6) 0.034(7) 0.021(7) C19 0.111(9) 0.034(5) 0.086(7) -0.006(5) 0.041(6) -0.001(5) N2A 0.113(9) 0.077(6) 0.100(8) 0.006(6) 0.050(7) -0.012(6) N3A 0.104(8) 0.056(6) 0.099(7) 0.015(5) 0.028(6) 0.031(6) O3A 0.123(10) 0.097(8) 0.42(3) 0.095(11) 0.156(15) 0.057(7) O4A 0.157(8) 0.071(5) 0.088(5) 0.018(4) 0.074(5) 0.058(5) O5A 0.103(6) 0.086(5) 0.072(5) 0.002(4) 0.025(4) -0.026(4) O6A 0.141(8) 0.119(7) 0.122(7) 0.004(6) 0.055(6) -0.061(7) 102A 0.24(3) 0.22(2) 0.128(15) 0.023(15) 0.098(18) -0.03(2) 101A 0.62(7) 0.41(5) 0.58(7) -0.35(5) 0.54(6) -0.46(5) C16 0.086(11) 0.017(7) 0.065(8) 0.001(6) 0.029(8) 0.000(7) C18 0.072(11) 0.037(9) 0.070(10) 0.005(7) 0.035(9) -0.006(7) C20 0.060(10) 0.030(8) 0.072(10) -0.007(7) 0.025(9) -0.001(7) N2B 0.095(13) 0.072(12) 0.060(9) -0.009(8) 0.005(9) -0.008(9) N3B 0.150(18) 0.087(13) 0.120(15) 0.004(11) 0.050(14) 0.012(13) O3B 0.61(6) 0.087(11) 0.59(6) 0.000 0.48(5) 0.000 O4B 0.142(15) 0.088(10) 0.181(16) -0.008(10) 0.122(13) -0.010(9) O5B 0.129(14) 0.067(10) 0.087(9) -0.011(7) 0.007(8) 0.016(8) O6B 0.092(11) 0.135(14) 0.099(10) -0.046(10) -0.001(9) 0.004(10) 102B 0.48(14) 0.29(9) 0.8(2) -0.20(12) -0.38(16) 0.25(10) 101B 0.20(4) 0.62(9) 0.36(6) 0.45(7) 0.23(4) 0.30(5) O9 0.148(6) 0.100(4) 0.119(5) -0.006(3) 0.060(4) -0.068(4) N5 0.086(5) 0.140(7) 0.142(7) 0.023(6) 0.039(5) -0.031(5) C100 0.177(13) 0.234(17) 0.161(11) -0.030(11) 0.072(10) -0.109(13) Zn1 0.0880(8) 0.0437(7) 0.0770(7) -0.0003(3) 0.0275(5) -0.0053(4) _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 N1 C20 1.414(15) . ? N1 C17 1.423(12) . ? N1 C19 1.486(10) . ? N1 C16 1.526(14) . ? N1 C18 1.528(15) . ? N1 C15 1.533(11) . ? N1 Zn1 2.078(5) . ? O1 C1 1.224(8) . ? O1 Zn1 2.370(5) . ? O2 C1 1.268(8) . ? O2 Zn1 2.025(4) . ? C9 C8 1.372(11) 4_544 ? C9 C10 1.414(10) . ? C9 N2B 1.596(18) 3_545 ? C4 C3 1.362(9) . ? C4 C5 1.378(10) . ? C4 H4 0.9300 . ? C5 C7 1.381(10) . ? C5 N3B 1.55(2) 6 ? C1 C3 1.521(9) . ? C1 Zn1 2.490(7) . ? C8 C9 1.372(11) 4_554 ? C8 C11 1.415(11) 4_554 ? C8 C7 1.485(9) . ? C2 C3 1.373(8) . ? C2 C6 1.402(9) . ? C2 H2 0.9300 . ? C10 C13 1.363(10) . ? C10 H10 0.9300 . ? C6 C7 1.393(10) . ? C6 N3A 1.527(13) . ? O7 C14 1.207(10) . ? O7 Zn1 2.000(6) . ? O8 C14 1.236(10) . ? C13 C12 1.352(11) . ? C13 C14 1.548(12) . ? C11 C12 1.366(11) . ? C11 C8 1.415(11) 4_544 ? C11 N2A 1.501(13) 2_554 ? C12 H12 0.9300 . ? C14 Zn1 2.566(10) . ? C15 C17 1.508(16) 2_655 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C15 1.508(16) 2_655 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C19 1.53(2) 2_655 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? N2A O5A 1.213(12) . ? N2A O6A 1.256(12) . ? N2A C11 1.501(13) 2_554 ? N3A O3A 1.182(14) . ? N3A O4A 1.196(12) . ? 102A N5 1.57(3) . ? 101A N5 1.28(2) . ? C16 C16 1.46(3) 2_655 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C20 1.55(2) 2_655 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C20 C18 1.55(2) 2_655 ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? N2B O5B 1.212(19) . ? N2B O6B 1.27(2) . ? N2B C9 1.596(18) 3_455 ? N3B O4B 1.23(2) . ? N3B C5 1.55(2) 6_556 ? N3B O3B 1.58(2) . ? O3B N3B 1.58(2) 2_655 ? O4B O4B 1.09(2) 2_655 ? 102B N5 1.86(9) . ? 101B N5 1.25(2) . ? O9 C100 1.040(15) . ? O9 Zn1 2.013(7) . ? N5 C100 1.276(16) . ? 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 C20 N1 C17 141.1(9) . . ? C20 N1 C19 52.8(7) . . ? C17 N1 C19 109.1(7) . . ? C20 N1 C16 110.7(9) . . ? C17 N1 C16 55.6(8) . . ? C19 N1 C16 137.0(8) . . ? C20 N1 C18 108.4(9) . . ? C17 N1 C18 53.1(8) . . ? C19 N1 C18 58.7(8) . . ? C16 N1 C18 104.5(9) . . ? C20 N1 C15 56.1(8) . . ? C17 N1 C15 109.2(7) . . ? C19 N1 C15 104.2(6) . . ? C16 N1 C15 57.2(8) . . ? C18 N1 C15 134.6(8) . . ? C20 N1 Zn1 109.8(7) . . ? C17 N1 Zn1 109.0(5) . . ? C19 N1 Zn1 112.1(5) . . ? C16 N1 Zn1 110.9(6) . . ? C18 N1 Zn1 112.4(6) . . ? C15 N1 Zn1 113.0(5) . . ? C1 O1 Zn1 80.9(4) . . ? C1 O2 Zn1 95.5(4) . . ? C8 C9 C10 118.6(7) 4_544 . ? C8 C9 N2B 128.8(8) 4_544 3_545 ? C10 C9 N2B 111.5(8) . 3_545 ? C3 C4 C5 121.3(6) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C7 122.2(7) . . ? C4 C5 N3B 105.1(10) . 6 ? C7 C5 N3B 132.4(10) . 6 ? O1 C1 O2 124.0(6) . . ? O1 C1 C3 119.3(6) . . ? O2 C1 C3 116.7(6) . . ? O1 C1 Zn1 70.0(4) . . ? O2 C1 Zn1 54.1(3) . . ? C3 C1 Zn1 170.4(5) . . ? C9 C8 C11 117.5(6) 4_554 4_554 ? C9 C8 C7 121.1(8) 4_554 . ? C11 C8 C7 121.3(7) 4_554 . ? C3 C2 C6 120.4(6) . . ? C3 C2 H2 119.8 . . ? C6 C2 H2 119.8 . . ? C13 C10 C9 121.8(7) . . ? C13 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C4 C3 C2 118.5(6) . . ? C4 C3 C1 119.7(6) . . ? C2 C3 C1 121.8(6) . . ? C7 C6 C2 121.4(6) . . ? C7 C6 N3A 128.8(7) . . ? C2 C6 N3A 109.8(7) . . ? C5 C7 C6 116.2(6) . . ? C5 C7 C8 121.0(6) . . ? C6 C7 C8 122.7(6) . . ? C14 O7 Zn1 103.5(6) . . ? C12 C13 C10 120.3(7) . . ? C12 C13 C14 119.6(8) . . ? C10 C13 C14 120.1(8) . . ? C12 C11 C8 122.9(8) . 4_544 ? C12 C11 N2A 108.7(9) . 2_554 ? C8 C11 N2A 128.3(7) 4_544 2_554 ? C13 C12 C11 119.0(9) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? O7 C14 O8 126.1(9) . . ? O7 C14 C13 115.5(9) . . ? O8 C14 C13 118.3(9) . . ? O7 C14 Zn1 49.3(5) . . ? O8 C14 Zn1 76.8(6) . . ? C13 C14 Zn1 164.5(7) . . ? C17 C15 N1 109.7(7) 2_655 . ? C17 C15 H15A 109.7 2_655 . ? N1 C15 H15A 109.7 . . ? C17 C15 H15B 109.7 2_655 . ? N1 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N1 C17 C15 112.5(8) . 2_655 ? N1 C17 H17A 109.1 . . ? C15 C17 H17A 109.1 2_655 . ? N1 C17 H17B 109.1 . . ? C15 C17 H17B 109.1 2_655 . ? H17A C17 H17B 107.8 . . ? N1 C19 C19 110.2(5) . 2_655 ? N1 C19 H19A 109.6 . . ? C19 C19 H19A 109.6 2_655 . ? N1 C19 H19B 109.6 . . ? C19 C19 H19B 109.6 2_655 . ? H19A C19 H19B 108.1 . . ? O5A N2A O6A 120.5(11) . . ? O5A N2A C11 115.1(9) . 2_554 ? O6A N2A C11 124.3(10) . 2_554 ? O3A N3A O4A 122.2(10) . . ? O3A N3A C6 123.8(9) . . ? O4A N3A C6 114.0(11) . . ? C16 C16 N1 111.1(6) 2_655 . ? C16 C16 H16A 109.4 2_655 . ? N1 C16 H16A 109.4 . . ? C16 C16 H16B 109.4 2_655 . ? N1 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N1 C18 C20 109.7(10) . 2_655 ? N1 C18 H18A 109.7 . . ? C20 C18 H18A 109.7 2_655 . ? N1 C18 H18B 109.7 . . ? C20 C18 H18B 109.7 2_655 . ? H18A C18 H18B 108.2 . . ? N1 C20 C18 111.5(11) . 2_655 ? N1 C20 H20A 109.3 . . ? C18 C20 H20A 109.3 2_655 . ? N1 C20 H20B 109.3 . . ? C18 C20 H20B 109.3 2_655 . ? H20A C20 H20B 108.0 . . ? O5B N2B O6B 118.5(17) . . ? O5B N2B C9 116.8(15) . 3_455 ? O6B N2B C9 124.8(15) . 3_455 ? O4B N3B C5 117.6(17) . 6_556 ? O4B N3B O3B 106.7(18) . . ? C5 N3B O3B 135.2(15) 6_556 . ? N3B O3B N3B 90.6(18) . 2_655 ? O4B O4B N3B 118.0(12) 2_655 . ? C100 O9 Zn1 138.2(11) . . ? 101B N5 C100 125.7(19) . . ? 101B N5 101A 64(4) . . ? C100 N5 101A 146.9(17) . . ? 101B N5 102A 113(2) . . ? C100 N5 102A 104.3(13) . . ? 101A N5 102A 98(2) . . ? 101B N5 102B 116(5) . . ? C100 N5 102B 92(5) . . ? 101A N5 102B 60(5) . . ? 102A N5 102B 101(3) . . ? O9 C100 N5 146.0(16) . . ? O7 Zn1 O9 101.5(3) . . ? O7 Zn1 O2 140.6(2) . . ? O9 Zn1 O2 97.3(2) . . ? O7 Zn1 N1 102.0(2) . . ? O9 Zn1 N1 97.6(2) . . ? O2 Zn1 N1 109.52(17) . . ? O7 Zn1 O1 95.5(2) . . ? O9 Zn1 O1 156.4(2) . . ? O2 Zn1 O1 59.47(17) . . ? N1 Zn1 O1 94.71(17) . . ? O7 Zn1 C1 118.7(2) . . ? O9 Zn1 C1 127.5(3) . . ? O2 Zn1 C1 30.46(19) . . ? N1 Zn1 C1 104.83(18) . . ? O1 Zn1 C1 29.05(18) . . ? O7 Zn1 C14 27.2(3) . . ? O9 Zn1 C14 96.5(3) . . ? O2 Zn1 C14 116.7(3) . . ? N1 Zn1 C14 129.2(3) . . ? O1 Zn1 C14 91.2(2) . . ? C1 Zn1 C14 104.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C4 C5 C7 -0.4(11) . . . . ? C3 C4 C5 N3B -175.5(9) . . . 6 ? Zn1 O1 C1 O2 4.1(6) . . . . ? Zn1 O1 C1 C3 -177.2(5) . . . . ? Zn1 O2 C1 O1 -4.7(7) . . . . ? Zn1 O2 C1 C3 176.5(4) . . . . ? C8 C9 C10 C13 -1.5(11) 4_544 . . . ? N2B C9 C10 C13 167.2(9) 3_545 . . . ? C5 C4 C3 C2 -0.3(10) . . . . ? C5 C4 C3 C1 179.1(6) . . . . ? C6 C2 C3 C4 1.2(9) . . . . ? C6 C2 C3 C1 -178.2(5) . . . . ? O1 C1 C3 C4 0.0(9) . . . . ? O2 C1 C3 C4 178.8(6) . . . . ? Zn1 C1 C3 C4 -164(2) . . . . ? O1 C1 C3 C2 179.4(6) . . . . ? O2 C1 C3 C2 -1.8(9) . . . . ? Zn1 C1 C3 C2 15(3) . . . . ? C3 C2 C6 C7 -1.5(10) . . . . ? C3 C2 C6 N3A 176.9(6) . . . . ? C4 C5 C7 C6 0.1(11) . . . . ? N3B C5 C7 C6 173.8(12) 6 . . . ? C4 C5 C7 C8 -176.7(7) . . . . ? N3B C5 C7 C8 -3.0(16) 6 . . . ? C2 C6 C7 C5 0.8(10) . . . . ? N3A C6 C7 C5 -177.3(8) . . . . ? C2 C6 C7 C8 177.5(6) . . . . ? N3A C6 C7 C8 -0.5(12) . . . . ? C9 C8 C7 C5 110.7(9) 4_554 . . . ? C11 C8 C7 C5 -64.7(9) 4_554 . . . ? C9 C8 C7 C6 -65.9(9) 4_554 . . . ? C11 C8 C7 C6 118.7(8) 4_554 . . . ? C9 C10 C13 C12 -0.2(11) . . . . ? C9 C10 C13 C14 179.0(6) . . . . ? C10 C13 C12 C11 0.9(12) . . . . ? C14 C13 C12 C11 -178.3(7) . . . . ? C8 C11 C12 C13 0.0(12) 4_544 . . . ? N2A C11 C12 C13 -177.8(7) 2_554 . . . ? Zn1 O7 C14 O8 0.7(11) . . . . ? Zn1 O7 C14 C13 -176.5(5) . . . . ? C12 C13 C14 O7 172.6(8) . . . . ? C10 C13 C14 O7 -6.6(11) . . . . ? C12 C13 C14 O8 -4.8(12) . . . . ? C10 C13 C14 O8 176.0(8) . . . . ? C12 C13 C14 Zn1 162.5(18) . . . . ? C10 C13 C14 Zn1 -17(2) . . . . ? C20 N1 C15 C17 -77.0(11) . . . 2_655 ? C17 N1 C15 C17 62.4(9) . . . 2_655 ? C19 N1 C15 C17 -54.1(10) . . . 2_655 ? C16 N1 C15 C17 83.1(11) . . . 2_655 ? C18 N1 C15 C17 5.7(15) . . . 2_655 ? Zn1 N1 C15 C17 -176.1(7) . . . 2_655 ? C20 N1 C17 C15 9.2(19) . . . 2_655 ? C19 N1 C17 C15 63.2(11) . . . 2_655 ? C16 N1 C17 C15 -71.3(11) . . . 2_655 ? C18 N1 C17 C15 81.8(11) . . . 2_655 ? C15 N1 C17 C15 -50.2(10) . . . 2_655 ? Zn1 N1 C17 C15 -174.0(8) . . . 2_655 ? C20 N1 C19 C19 91.2(13) . . . 2_655 ? C17 N1 C19 C19 -49.2(13) . . . 2_655 ? C16 N1 C19 C19 10.6(19) . . . 2_655 ? C18 N1 C19 C19 -66.6(12) . . . 2_655 ? C15 N1 C19 C19 67.3(13) . . . 2_655 ? Zn1 N1 C19 C19 -170.1(9) . . . 2_655 ? C7 C6 N3A O3A 159.6(15) . . . . ? C2 C6 N3A O3A -18.6(17) . . . . ? C7 C6 N3A O4A -19.7(13) . . . . ? C2 C6 N3A O4A 162.1(8) . . . . ? C20 N1 C16 C16 -50.5(19) . . . 2_655 ? C17 N1 C16 C16 88.0(18) . . . 2_655 ? C19 N1 C16 C16 7(2) . . . 2_655 ? C18 N1 C16 C16 66.1(18) . . . 2_655 ? C15 N1 C16 C16 -68.1(16) . . . 2_655 ? Zn1 N1 C16 C16 -172.6(14) . . . 2_655 ? C20 N1 C18 C20 61.7(11) . . . 2_655 ? C17 N1 C18 C20 -79.1(12) . . . 2_655 ? C19 N1 C18 C20 80.2(11) . . . 2_655 ? C16 N1 C18 C20 -56.4(13) . . . 2_655 ? C15 N1 C18 C20 1.5(17) . . . 2_655 ? Zn1 N1 C18 C20 -176.7(9) . . . 2_655 ? C17 N1 C20 C18 -1(2) . . . 2_655 ? C19 N1 C20 C18 -75.0(12) . . . 2_655 ? C16 N1 C20 C18 59.1(14) . . . 2_655 ? C18 N1 C20 C18 -55.0(12) . . . 2_655 ? C15 N1 C20 C18 76.9(12) . . . 2_655 ? Zn1 N1 C20 C18 -178.2(9) . . . 2_655 ? O4B N3B O3B N3B 0.3(11) . . . 2_655 ? C5 N3B O3B N3B 173(3) 6_556 . . 2_655 ? C5 N3B O4B O4B -175(2) 6_556 . . 2_655 ? O3B N3B O4B O4B -1(4) . . . 2_655 ? Zn1 O9 C100 N5 160(2) . . . . ? 101B N5 C100 O9 -88(6) . . . . ? 101A N5 C100 O9 176(6) . . . . ? 102A N5 C100 O9 45(4) . . . . ? 102B N5 C100 O9 147(4) . . . . ? C14 O7 Zn1 O9 81.7(6) . . . . ? C14 O7 Zn1 O2 -35.2(7) . . . . ? C14 O7 Zn1 N1 -177.9(5) . . . . ? C14 O7 Zn1 O1 -81.9(5) . . . . ? C14 O7 Zn1 C1 -63.4(6) . . . . ? C100 O9 Zn1 O7 -7.5(17) . . . . ? C100 O9 Zn1 O2 137.6(17) . . . . ? C100 O9 Zn1 N1 -111.4(17) . . . . ? C100 O9 Zn1 O1 127.8(16) . . . . ? C100 O9 Zn1 C1 133.2(16) . . . . ? C100 O9 Zn1 C14 19.6(17) . . . . ? C1 O2 Zn1 O7 -54.9(5) . . . . ? C1 O2 Zn1 O9 -173.1(4) . . . . ? C1 O2 Zn1 N1 86.2(4) . . . . ? C1 O2 Zn1 O1 2.4(3) . . . . ? C1 O2 Zn1 C14 -72.1(4) . . . . ? C20 N1 Zn1 O7 -149.3(7) . . . . ? C17 N1 Zn1 O7 32.9(6) . . . . ? C19 N1 Zn1 O7 153.8(6) . . . . ? C16 N1 Zn1 O7 -26.7(7) . . . . ? C18 N1 Zn1 O7 89.9(7) . . . . ? C15 N1 Zn1 O7 -88.7(6) . . . . ? C20 N1 Zn1 O9 -45.8(7) . . . . ? C17 N1 Zn1 O9 136.4(6) . . . . ? C19 N1 Zn1 O9 -102.6(6) . . . . ? C16 N1 Zn1 O9 76.9(7) . . . . ? C18 N1 Zn1 O9 -166.6(7) . . . . ? C15 N1 Zn1 O9 14.8(6) . . . . ? C20 N1 Zn1 O2 54.8(7) . . . . ? C17 N1 Zn1 O2 -123.1(6) . . . . ? C19 N1 Zn1 O2 -2.1(6) . . . . ? C16 N1 Zn1 O2 177.4(7) . . . . ? C18 N1 Zn1 O2 -66.0(7) . . . . ? C15 N1 Zn1 O2 115.4(5) . . . . ? C20 N1 Zn1 O1 114.0(7) . . . . ? C17 N1 Zn1 O1 -63.8(6) . . . . ? C19 N1 Zn1 O1 57.2(6) . . . . ? C16 N1 Zn1 O1 -123.3(7) . . . . ? C18 N1 Zn1 O1 -6.8(7) . . . . ? C15 N1 Zn1 O1 174.6(5) . . . . ? C20 N1 Zn1 C1 86.3(7) . . . . ? C17 N1 Zn1 C1 -91.5(6) . . . . ? C19 N1 Zn1 C1 29.5(6) . . . . ? C16 N1 Zn1 C1 -151.0(7) . . . . ? C18 N1 Zn1 C1 -34.5(7) . . . . ? C15 N1 Zn1 C1 146.9(5) . . . . ? C20 N1 Zn1 C14 -150.5(7) . . . . ? C17 N1 Zn1 C14 31.6(7) . . . . ? C19 N1 Zn1 C14 152.6(6) . . . . ? C16 N1 Zn1 C14 -27.9(8) . . . . ? C18 N1 Zn1 C14 88.6(7) . . . . ? C15 N1 Zn1 C14 -89.9(6) . . . . ? C1 O1 Zn1 O7 145.1(4) . . . . ? C1 O1 Zn1 O9 8.8(7) . . . . ? C1 O1 Zn1 O2 -2.5(4) . . . . ? C1 O1 Zn1 N1 -112.4(4) . . . . ? C1 O1 Zn1 C14 118.2(4) . . . . ? O1 C1 Zn1 O7 -40.5(5) . . . . ? O2 C1 Zn1 O7 143.6(4) . . . . ? C3 C1 Zn1 O7 125(2) . . . . ? O1 C1 Zn1 O9 -175.5(4) . . . . ? O2 C1 Zn1 O9 8.6(5) . . . . ? C3 C1 Zn1 O9 -10(3) . . . . ? O1 C1 Zn1 O2 175.8(6) . . . . ? C3 C1 Zn1 O2 -19(2) . . . . ? O1 C1 Zn1 N1 72.4(4) . . . . ? O2 C1 Zn1 N1 -103.4(4) . . . . ? C3 C1 Zn1 N1 -122(3) . . . . ? O2 C1 Zn1 O1 -175.8(6) . . . . ? C3 C1 Zn1 O1 165(3) . . . . ? O1 C1 Zn1 C14 -65.5(4) . . . . ? O2 C1 Zn1 C14 118.7(4) . . . . ? C3 C1 Zn1 C14 100(3) . . . . ? O8 C14 Zn1 O7 -179.4(9) . . . . ? C13 C14 Zn1 O7 12.1(18) . . . . ? O7 C14 Zn1 O9 -102.6(6) . . . . ? O8 C14 Zn1 O9 78.0(6) . . . . ? C13 C14 Zn1 O9 -91(2) . . . . ? O7 C14 Zn1 O2 155.8(5) . . . . ? O8 C14 Zn1 O2 -23.6(6) . . . . ? C13 C14 Zn1 O2 168(2) . . . . ? O7 C14 Zn1 N1 2.6(7) . . . . ? O8 C14 Zn1 N1 -176.8(5) . . . . ? C13 C14 Zn1 N1 15(2) . . . . ? O7 C14 Zn1 O1 99.7(5) . . . . ? O8 C14 Zn1 O1 -79.7(5) . . . . ? C13 C14 Zn1 O1 112(2) . . . . ? O7 C14 Zn1 C1 125.9(5) . . . . ? O8 C14 Zn1 C1 -53.5(6) . . . . ? C13 C14 Zn1 C1 138(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 50.31 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.630 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 942880' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_BMOF-1-bpdc-[NO2]2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BMOF-1-bpdc-[NO2]2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H0 N8 O17 Zn2' _chemical_formula_weight 1091.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fmmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 28.0614(11) _cell_length_b 30.0942(19) _cell_length_c 30.0947(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25415(2) _cell_formula_units_Z 16 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 4.16 _cell_measurement_theta_max 67.34 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_max 0.60 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8640 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7845 _exptl_absorpt_correction_T_max 0.8345 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _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 36215 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 82.01 _reflns_number_total 6067 _reflns_number_gt 4670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The structure was refined using twin law (0 1 0, 1 0 0. 0 -1 2) and BASF value is 0.15954. Due to the twinned structure, the bpdc-[NO2]2 was refined as disordered over two different position. In addition, the 4,4'- bpy is also refined as disordered. Due to the severely disordered structure, no hydrogen atom was added (refine unstable). Squeeze was used to remove electron density from unrefined nitro groups, hydrogen and solvent molecule. High wR2 value is due to the quality of the structure. We have tried our best to resolve any disorders of the twinned structure. The high residual electron density may be due to the electron denstiy of unresolved nitro groups, solvents that SQUEEZE may not able to remove from the structure. The following atoms were refined isotropically due to the twin/disordered: C7, C8, C10, C13, c14, c15, o7, o9, o8, o5a, o6a, n5, C16a, C17a, C22a, C23a, C30a, C31a, o5b, o6b, C16b, c17b, c22b, c23b, c30b, c31b, c21, c34, c36, n6, c11. ; 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 0.000 0.000 0.000 1004 407 ' ' 2 0.500 0.000 0.500 1004 407 ' ' 3 0.432 0.137 -0.005 1625 767 ' ' 4 -0.006 0.363 0.082 1626 756 ' ' 5 0.500 0.500 0.000 1004 407 ' ' 6 0.000 0.500 0.500 1004 407 ' ' 7 0.067 0.637 -0.005 1625 767 ' ' 8 0.494 0.863 0.082 1625 756 ' ' _platon_squeeze_details ? _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^)+(0.5962P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6067 _refine_ls_number_parameters 283 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_gt 0.1579 _refine_ls_wR_factor_ref 0.5968 _refine_ls_wR_factor_gt 0.5586 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.009 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 O1 O 0.0000 0.93390(18) 0.28663(18) 0.0438(12) Uani 1 2 d S . . O2 O -0.06630(19) 1.0000 0.29105(18) 0.0454(12) Uani 1 2 d S . . O3 O 0.2371(3) 0.31501(14) 0.03772(18) 0.0770(16) Uani 1 1 d . . . O4 O 0.31490(15) 0.2638(3) 0.03967(17) 0.0847(18) Uani 1 1 d . . . N1 N 0.0000 1.0000 0.3753(5) 0.035(3) Uani 1 4 d S . . N3 N 0.2500 0.2500 0.1253(5) 0.041(3) Uani 1 2 d S . . N2 N 0.0000 1.0000 0.1255(5) 0.036(2) Uani 1 4 d S . . C1 C 0.3330(2) 0.2628(3) 0.0000 0.0384(15) Uani 1 2 d S . . C2 C 0.2285(4) 0.3834(3) 0.0000 0.052(2) Uani 1 2 d S . . C3 C -0.0173(4) 0.9160(4) 0.2486(3) 0.109(3) Uiso 1 1 d . . . C4 C 0.3849(3) 0.2695(2) 0.0000 0.0421(16) Uani 1 2 d S . . C5 C 0.2358(2) 0.3334(2) 0.0000 0.0376(15) Uani 1 2 d S . . C6 C -0.0232(5) 0.8688(4) 0.2510(5) 0.119(4) Uani 1 1 d . . . C7 C -0.0834(4) 0.9843(4) 0.2524(3) 0.103(3) Uiso 1 1 d . . . C8 C -0.1351(4) 0.9792(3) 0.2511(3) 0.089(2) Uiso 1 1 d D . . C10 C 0.0000 0.9645(5) 0.1015(4) 0.081(3) Uiso 1 2 d S . . C12 C 0.0000 0.8426(4) 0.2861(5) 0.078(3) Uani 1 2 d S . . C13 C -0.0336(6) 0.7706(5) 0.2512(6) 0.140(5) Uiso 1 1 d . . . C14 C 0.0000 0.7974(7) 0.2883(6) 0.114(5) Uiso 1 2 d S . . C15 C -0.0527(6) 0.8015(5) 0.2171(5) 0.127(4) Uiso 1 1 d . A . C20 C 0.0000 1.0000 0.0268(6) 0.053(5) Uani 1 4 d S . . C18 C 0.2161(3) 0.4759(3) 0.0000 0.0502(18) Uani 1 2 d S . . C19 C 0.0000 0.9626(4) 0.0540(3) 0.103(6) Uani 1 2 d S . . C24 C 0.2500 0.2500 0.2223(5) 0.043(3) Uani 1 2 d S . . C29 C 0.0000 1.0000 0.4733(5) 0.040(3) Uani 1 4 d S . . C28 C 0.0404(5) 1.0000 0.4489(4) 0.070(3) Uiso 1 2 d S . . C26 C -0.1587(4) 1.0000 0.2875(3) 0.080(4) Uani 1 2 d SD . . C27 C -0.1530(4) 0.9560(4) 0.2144(3) 0.097(3) Uani 1 1 d D . . O7 O 0.1496(4) 0.5000 -0.0666(4) 0.103(3) Uiso 1 2 d S . . O9 O -0.1010(10) 0.7444(11) 0.1854(8) 0.279(9) Uiso 1 1 d . A . N5 N 0.1720(6) 0.4655(6) -0.0749(5) 0.150(4) Uiso 1 1 d . . . O8 O 0.1757(11) 0.4485(10) -0.1152(9) 0.293(10) Uiso 1 1 d . A . C33 C 0.4749(4) 0.2790(4) 0.0000 0.071(3) Uani 1 2 d S . . C35 C -0.2054(4) 1.0000 0.2853(4) 0.097(5) Uani 1 2 d SD . . O10 O -0.0635(15) 0.8049(13) 0.1529(12) 0.359(17) Uiso 1 1 d . A . N4 N -0.0839(8) 0.7847(9) 0.1793(7) 0.190(7) Uiso 1 1 d . . . O5A O 0.0000 0.850(5) 0.113(4) 0.71(7) Uiso 1.063(14) 2 d SP A 2 O6A O -0.0310(16) 1.0000 0.1925(12) 0.38(2) Uiso 1.063(14) 2 d SP A 2 C16A C 0.2090(6) 0.4036(5) -0.0353(5) 0.078(4) Uiso 0.531(7) 1 d P A 2 C17A C 0.1994(4) 0.4488(4) -0.0347(4) 0.057(3) Uiso 0.531(7) 1 d P A 2 C22A C 0.2164(6) 0.2442(6) 0.1495(6) 0.083(4) Uiso 0.531(7) 1 d P . 2 C23A C 0.2089(5) 0.2476(4) 0.1984(4) 0.059(3) Uiso 0.531(7) 1 d P A 2 C30A C 0.4024(4) 0.2947(4) 0.0354(4) 0.060(3) Uiso 0.531(7) 1 d P A 2 C31A C 0.4495(5) 0.2967(5) 0.0360(5) 0.072(3) Uiso 0.531(7) 1 d P A 2 O5B O -0.0220(2) 0.9357(2) 0.2099(2) 0.0364(16) Uiso 0.469(7) 1 d P . 1 O6B O -0.0634(2) 0.9768(2) 0.2137(2) 0.0326(15) Uiso 0.469(7) 1 d P . 1 C16B C 0.2446(5) 0.4061(5) -0.0400(5) 0.055(3) Uiso 0.469(7) 1 d P A 1 C17B C 0.2377(5) 0.4552(5) -0.0380(5) 0.064(3) Uiso 0.469(7) 1 d P A 1 C22B C 0.2570(4) 0.2835(5) 0.1472(5) 0.055(3) Uiso 0.469(7) 1 d P . 1 C23B C 0.2316(4) 0.2129(4) 0.1978(4) 0.053(3) Uiso 0.469(7) 1 d P . 1 C30B C 0.4086(5) 0.2557(5) 0.0391(5) 0.060(3) Uiso 0.469(7) 1 d P . 1 C31B C 0.4575(10) 0.2577(10) 0.0297(9) 0.108(7) Uiso 0.469(7) 1 d P . 1 C21 C 0.0369(4) 1.0000 0.3986(4) 0.068(2) Uiso 1 2 d S . . C34 C -0.1980(4) 0.9513(4) 0.2156(4) 0.103(3) Uiso 1 1 d D A . C36 C -0.2213(5) 0.9693(5) 0.2520(4) 0.129(4) Uiso 1 1 d D . . N6 N -0.193(3) 0.917(2) 0.166(2) 0.52(3) Uiso 1 1 d . . . C11 C -0.0496(3) 0.8478(3) 0.2148(2) 0.0694(17) Uiso 1 1 d . . . Zn1 Zn 0.0000 1.0000 0.19800(5) 0.0333(8) Uani 1 4 d S . . Zn3 Zn 0.0000 1.0000 0.30270(5) 0.0332(8) Uani 1 4 d S . . Zn2 Zn 0.2500 0.2500 0.05223(5) 0.0324(8) 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 O1 0.054(2) 0.039(3) 0.038(3) -0.0023(18) 0.000 0.000 O2 0.040(2) 0.062(3) 0.034(2) 0.000 -0.0079(19) 0.000 O3 0.145(5) 0.030(2) 0.056(3) 0.0019(17) 0.002(3) 0.026(2) O4 0.0324(18) 0.176(6) 0.046(2) 0.002(3) 0.0113(17) -0.016(2) N1 0.010(3) 0.068(8) 0.026(5) 0.000 0.000 0.000 N3 0.016(4) 0.079(8) 0.029(5) 0.000 0.000 0.0044(19) N2 0.030(5) 0.055(7) 0.021(5) 0.000 0.000 0.000 C1 0.034(3) 0.042(3) 0.038(3) 0.000 0.000 0.005(2) C2 0.065(5) 0.039(4) 0.053(5) 0.000 0.000 0.020(4) C4 0.041(3) 0.038(3) 0.047(3) 0.000 0.000 0.012(2) C5 0.032(2) 0.033(3) 0.048(4) 0.000 0.000 0.0030(19) C6 0.103(7) 0.099(7) 0.156(10) -0.026(7) 0.006(6) -0.025(6) C12 0.072(6) 0.061(5) 0.099(8) 0.009(5) 0.000 0.000 C20 0.087(12) 0.041(8) 0.031(9) 0.000 0.000 0.000 C18 0.046(3) 0.041(4) 0.064(4) 0.000 0.000 0.008(3) C19 0.210(18) 0.053(5) 0.045(4) -0.014(3) 0.000 0.000 C24 0.055(7) 0.043(7) 0.030(8) 0.000 0.000 -0.003(3) C29 0.037(6) 0.056(8) 0.026(8) 0.000 0.000 0.000 C26 0.047(4) 0.150(12) 0.042(4) 0.000 0.000(3) 0.000 C27 0.078(4) 0.115(7) 0.097(5) -0.008(5) 0.006(4) 0.001(4) C33 0.056(5) 0.080(6) 0.077(6) 0.000 0.000 -0.002(4) C35 0.041(4) 0.172(15) 0.078(6) 0.000 -0.013(4) 0.000 Zn1 0.0328(13) 0.0414(15) 0.0257(15) 0.000 0.000 0.000 Zn3 0.0296(13) 0.0450(16) 0.0248(14) 0.000 0.000 0.000 Zn2 0.0333(13) 0.0376(14) 0.0261(14) 0.000 0.000 0.0007(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 O1 C3 1.354(12) . ? O1 C3 1.354(12) 20 ? O1 Zn3 2.047(5) . ? O2 C7 1.343(11) 19_575 ? O2 C7 1.343(11) . ? O2 Zn3 1.893(5) . ? O3 C5 1.263(6) . ? O3 Zn2 2.037(4) . ? O4 C1 1.298(6) . ? O4 Zn2 1.906(4) . ? N1 C21 1.249(14) . ? N1 C21 1.249(14) 2_575 ? N1 Zn3 2.186(15) . ? N3 C22A 1.20(2) 14 ? N3 C22A 1.20(2) . ? N3 C22B 1.218(15) 14 ? N3 C22B 1.218(15) . ? N3 Zn2 2.200(15) . ? N2 C10 1.290(16) . ? N2 C10 1.290(16) 2_575 ? N2 Zn1 2.182(15) . ? C1 O4 1.298(6) 18 ? C1 C4 1.468(9) . ? C2 C16A 1.341(17) . ? C2 C16A 1.341(17) 18 ? C2 C16B 1.456(16) . ? C2 C16B 1.456(16) 18 ? C2 C5 1.519(10) . ? C3 C3 0.97(2) 20 ? C3 O5B 1.314(13) . ? C3 C6 1.432(17) . ? C3 O5B 1.709(13) 20 ? C3 C6 1.820(16) 20 ? C4 C30A 1.399(13) 18 ? C4 C30A 1.399(13) . ? C4 C30B 1.413(15) 18 ? C4 C30B 1.413(15) . ? C5 O3 1.263(6) 18 ? C6 C6 1.30(3) 20 ? C6 C11 1.461(14) . ? C6 C12 1.470(19) . ? C6 C3 1.820(16) 20 ? C7 C7 0.94(2) 19_575 ? C7 O6B 1.312(11) . ? C7 C8 1.458(14) . ? C7 O6B 1.744(12) 19_575 ? C7 C8 1.819(14) 19_575 ? C8 C8 1.253(19) 19_575 ? C8 C27 1.399(11) . ? C8 C26 1.427(11) . ? C8 C7 1.819(14) 19_575 ? C10 C19 1.432(16) . ? C12 C14 1.36(2) . ? C12 C6 1.470(19) 20 ? C13 C13 1.24(3) 8_565 ? C13 C15 1.48(2) . ? C13 C14 1.67(2) . ? C13 C13 1.89(3) 20 ? C14 C13 1.67(2) 20 ? C15 C11 1.396(18) . ? C15 N4 1.52(2) . ? C20 C19 1.391(15) 2_575 ? C20 C19 1.391(15) . ? C20 C20 1.61(4) 17_575 ? C18 C17A 1.404(13) . ? C18 C17A 1.404(13) 18 ? C18 C17B 1.436(16) 18 ? C18 C17B 1.436(16) . ? C18 C18 1.452(15) 19_565 ? C24 C23A 1.362(16) . ? C24 C23A 1.362(16) 14 ? C24 C23B 1.434(15) . ? C24 C23B 1.434(15) 14 ? C24 C24 1.67(3) 11 ? C29 C28 1.349(16) 2_575 ? C29 C28 1.349(16) . ? C29 C29 1.61(3) 17_576 ? C28 C21 1.519(17) . ? C26 C35 1.310(13) . ? C26 C8 1.427(11) 19_575 ? C27 C34 1.270(16) . ? O7 N5 1.239(19) . ? O7 N5 1.239(19) 19_565 ? O9 N4 1.32(3) . ? N5 O8 1.32(3) . ? N5 C17A 1.518(19) . ? C33 C31B 1.20(3) 18 ? C33 C31B 1.20(3) . ? C33 C33 1.41(2) 3_655 ? C33 C31A 1.402(16) . ? C33 C31A 1.402(16) 18 ? C35 C36 1.433(13) 19_575 ? C35 C36 1.433(13) . ? O10 N4 1.15(4) . ? O6A Zn1 0.88(5) . ? C16A C17A 1.39(2) . ? C22A C23A 1.49(2) . ? C22A C22A 1.92(4) 14 ? C30A C31A 1.323(19) . ? O5B O5B 1.233(14) 20 ? O5B C3 1.709(13) 20 ? O5B O6B 1.702(8) . ? O5B Zn1 2.063(7) . ? O6B O6B 1.398(13) 19_575 ? O6B C7 1.744(12) 19_575 ? O6B Zn1 1.970(6) . ? C16B C17B 1.49(2) . ? C22B C23B 1.561(18) 14 ? C23B C22B 1.561(18) 14 ? C30B C31B 1.40(3) . ? C31B C31B 1.79(5) 18 ? C34 C36 1.387(13) . ? C34 N6 1.83(6) . ? C36 C36 1.62(3) 11_455 ? C36 C36 1.85(3) 19_575 ? Zn1 O6A 0.88(5) 2_575 ? Zn1 O6B 1.970(6) 2_575 ? Zn1 O6B 1.970(6) 19_575 ? Zn1 O6B 1.970(6) 20 ? Zn1 O5B 2.063(7) 19_575 ? Zn1 O5B 2.063(7) 2_575 ? Zn1 O5B 2.063(7) 20 ? Zn1 Zn3 3.151(3) . ? Zn3 O2 1.893(5) 2_575 ? Zn3 O1 2.047(5) 2_575 ? Zn2 O4 1.906(4) 14 ? Zn2 O3 2.037(4) 14 ? Zn2 Zn2 3.143(3) 29 ? 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 C3 O1 C3 41.9(9) . 20 ? C3 O1 Zn3 125.9(6) . . ? C3 O1 Zn3 125.9(6) 20 . ? C7 O2 C7 41.2(10) 19_575 . ? C7 O2 Zn3 120.8(6) 19_575 . ? C7 O2 Zn3 120.8(6) . . ? C5 O3 Zn2 128.2(4) . . ? C1 O4 Zn2 123.5(4) . . ? C21 N1 C21 111.8(15) . 2_575 ? C21 N1 Zn3 124.1(7) . . ? C21 N1 Zn3 124.1(7) 2_575 . ? C22A N3 C22A 106(2) 14 . ? C22A N3 C22B 85.3(12) 14 14 ? C22A N3 C22B 55.2(10) . 14 ? C22A N3 C22B 55.2(10) 14 . ? C22A N3 C22B 85.3(12) . . ? C22B N3 C22B 114.7(17) 14 . ? C22A N3 Zn2 127.2(10) 14 . ? C22A N3 Zn2 127.2(10) . . ? C22B N3 Zn2 122.6(9) 14 . ? C22B N3 Zn2 122.6(9) . . ? C10 N2 C10 112.0(16) . 2_575 ? C10 N2 Zn1 124.0(8) . . ? C10 N2 Zn1 124.0(8) 2_575 . ? O4 C1 O4 133.8(7) 18 . ? O4 C1 C4 112.7(3) 18 . ? O4 C1 C4 112.7(3) . . ? C16A C2 C16A 104.9(15) . 18 ? C16A C2 C16B 42.1(8) . . ? C16A C2 C16B 124.7(10) 18 . ? C16A C2 C16B 124.7(10) . 18 ? C16A C2 C16B 42.1(8) 18 18 ? C16B C2 C16B 111.7(13) . 18 ? C16A C2 C5 120.3(8) . . ? C16A C2 C5 120.3(8) 18 . ? C16B C2 C5 115.0(6) . . ? C16B C2 C5 115.0(6) 18 . ? C3 C3 O5B 95.8(6) 20 . ? C3 C3 O1 69.0(5) 20 . ? O5B C3 O1 127.3(10) . . ? C3 C3 C6 96.7(7) 20 . ? O5B C3 C6 118.6(11) . . ? O1 C3 C6 113.2(11) . . ? C3 C3 O5B 49.9(4) 20 20 ? O5B C3 O5B 45.9(6) . 20 ? O1 C3 O5B 102.0(7) . 20 ? C6 C3 O5B 116.9(10) . 20 ? C3 C3 C6 51.4(6) 20 20 ? O5B C3 C6 116.7(10) . 20 ? O1 C3 C6 93.1(8) . 20 ? C6 C3 C6 45.3(10) . 20 ? O5B C3 C6 84.0(8) 20 20 ? C30A C4 C30A 99.4(11) 18 . ? C30A C4 C30B 50.1(8) 18 18 ? C30A C4 C30B 128.9(10) . 18 ? C30A C4 C30B 128.9(10) 18 . ? C30A C4 C30B 50.1(8) . . ? C30B C4 C30B 112.6(13) 18 . ? C30A C4 C1 115.0(6) 18 . ? C30A C4 C1 115.0(6) . . ? C30B C4 C1 115.3(7) 18 . ? C30B C4 C1 115.3(7) . . ? O3 C5 O3 128.0(7) 18 . ? O3 C5 C2 115.9(3) 18 . ? O3 C5 C2 115.9(3) . . ? C6 C6 C11 120.5(6) 20 . ? C6 C6 C3 83.3(7) 20 . ? C11 C6 C3 116.9(13) . . ? C6 C6 C12 63.7(6) 20 . ? C11 C6 C12 121.8(10) . . ? C3 C6 C12 121.1(11) . . ? C6 C6 C3 51.4(6) 20 20 ? C11 C6 C3 128.7(11) . 20 ? C3 C6 C3 31.9(8) . 20 ? C12 C6 C3 99.8(9) . 20 ? C7 C7 O6B 100.0(6) 19_575 . ? C7 C7 O2 69.4(5) 19_575 . ? O6B C7 O2 132.5(10) . . ? C7 C7 C8 96.1(6) 19_575 . ? O6B C7 C8 112.5(9) . . ? O2 C7 C8 114.6(8) . . ? C7 C7 O6B 47.8(4) 19_575 19_575 ? O6B C7 O6B 52.1(6) . 19_575 ? O2 C7 O6B 103.1(7) . 19_575 ? C8 C7 O6B 111.9(8) . 19_575 ? C7 C7 C8 52.8(5) 19_575 19_575 ? O6B C7 C8 115.2(8) . 19_575 ? O2 C7 C8 95.3(7) . 19_575 ? C8 C7 C8 43.2(7) . 19_575 ? O6B C7 C8 80.6(6) 19_575 19_575 ? C8 C8 C27 119.9(6) 19_575 . ? C8 C8 C26 63.9(4) 19_575 . ? C27 C8 C26 131.2(9) . . ? C8 C8 C7 83.9(6) 19_575 . ? C27 C8 C7 115.6(8) . . ? C26 C8 C7 113.3(9) . . ? C8 C8 C7 52.8(5) 19_575 19_575 ? C27 C8 C7 127.2(8) . 19_575 ? C26 C8 C7 95.1(7) . 19_575 ? C7 C8 C7 31.1(8) . 19_575 ? N2 C10 C19 126.2(12) . . ? C14 C12 C6 124.8(12) . . ? C14 C12 C6 124.8(12) . 20 ? C6 C12 C6 52.6(11) . 20 ? C13 C13 C15 126(2) 8_565 . ? C13 C13 C14 121.4(17) 8_565 . ? C15 C13 C14 111.2(13) . . ? C13 C13 C13 89.998(5) 8_565 20 ? C15 C13 C13 111.2(9) . 20 ? C14 C13 C13 55.6(7) . 20 ? C12 C14 C13 116.8(13) . . ? C12 C14 C13 116.8(13) . 20 ? C13 C14 C13 68.8(14) . 20 ? C11 C15 C13 129.6(13) . . ? C11 C15 N4 109.3(15) . . ? C13 C15 N4 121.0(17) . . ? C19 C20 C19 108.0(14) 2_575 . ? C19 C20 C20 126.0(7) 2_575 17_575 ? C19 C20 C20 126.0(7) . 17_575 ? C17A C18 C17A 96.1(11) . 18 ? C17A C18 C17B 118.8(9) . 18 ? C17A C18 C17B 45.4(8) 18 18 ? C17A C18 C17B 45.4(8) . . ? C17A C18 C17B 118.8(9) 18 . ? C17B C18 C17B 105.6(13) 18 . ? C17A C18 C18 125.4(5) . 19_565 ? C17A C18 C18 125.4(5) 18 19_565 ? C17B C18 C18 115.7(7) 18 19_565 ? C17B C18 C18 115.6(7) . 19_565 ? C20 C19 C10 123.7(11) . . ? C23A C24 C23A 116.0(16) . 14 ? C23A C24 C23B 51.8(8) . . ? C23A C24 C23B 94.3(10) 14 . ? C23A C24 C23B 94.3(10) . 14 ? C23A C24 C23B 51.8(8) 14 14 ? C23B C24 C23B 118.1(14) . 14 ? C23A C24 C24 122.0(8) . 11 ? C23A C24 C24 122.0(8) 14 11 ? C23B C24 C24 121.0(7) . 11 ? C23B C24 C24 121.0(7) 14 11 ? C28 C29 C28 114.3(16) 2_575 . ? C28 C29 C29 122.8(8) 2_575 17_576 ? C28 C29 C29 122.8(8) . 17_576 ? C29 C28 C21 119.1(12) . . ? C35 C26 C8 115.1(9) . 19_575 ? C35 C26 C8 115.1(9) . . ? C8 C26 C8 52.1(8) 19_575 . ? C34 C27 C8 113.0(10) . . ? N5 O7 N5 114.0(18) . 19_565 ? O7 N5 O8 123.3(19) . . ? O7 N5 C17A 111.9(13) . . ? O8 N5 C17A 124.3(19) . . ? C31B C33 C31B 96(3) 18 . ? C31B C33 C33 114.0(14) 18 3_655 ? C31B C33 C33 114.0(14) . 3_655 ? C31B C33 C31A 124.6(16) 18 . ? C31B C33 C31A 54.7(14) . . ? C33 C33 C31A 120.6(7) 3_655 . ? C31B C33 C31A 54.7(14) 18 18 ? C31B C33 C31A 124.6(16) . 18 ? C33 C33 C31A 120.6(7) 3_655 18 ? C31A C33 C31A 101.1(14) . 18 ? C26 C35 C36 110.4(9) . 19_575 ? C26 C35 C36 110.4(9) . . ? C36 C35 C36 80.2(13) 19_575 . ? O10 N4 O9 140(3) . . ? O10 N4 C15 93(3) . . ? O9 N4 C15 114(2) . . ? C2 C16A C17A 120.9(13) . . ? C16A C17A C18 120.9(11) . . ? C16A C17A N5 114.3(12) . . ? C18 C17A N5 124.8(11) . . ? N3 C22A C23A 134.3(16) . . ? N3 C22A C22A 37.2(10) . 14 ? C23A C22A C22A 97.3(9) . 14 ? C24 C23A C22A 114.0(13) . . ? C31A C30A C4 112.7(11) . . ? C30A C31A C33 118.8(13) . . ? O5B O5B C3 84.2(6) 20 . ? O5B O5B C3 49.9(4) 20 20 ? C3 O5B C3 34.4(8) . 20 ? O5B O5B O6B 133.1(3) 20 . ? C3 O5B O6B 109.6(7) . . ? C3 O5B O6B 130.2(6) 20 . ? O5B O5B Zn1 72.61(19) 20 . ? C3 O5B Zn1 123.1(7) . . ? C3 O5B Zn1 104.5(5) 20 . ? O6B O5B Zn1 62.2(3) . . ? C7 O6B O6B 80.1(6) . 19_575 ? C7 O6B O5B 118.6(7) . . ? O6B O6B O5B 136.6(3) 19_575 . ? C7 O6B C7 32.2(8) . 19_575 ? O6B O6B C7 47.8(4) 19_575 19_575 ? O5B O6B C7 138.9(6) . 19_575 ? C7 O6B Zn1 122.6(6) . . ? O6B O6B Zn1 69.22(18) 19_575 . ? O5B O6B Zn1 67.9(3) . . ? C7 O6B Zn1 102.3(5) 19_575 . ? C17B C16B C2 113.0(11) . . ? C18 C17B C16B 121.1(12) . . ? N3 C22B C23B 128.1(13) . 14 ? C24 C23B C22B 111.9(10) . 14 ? C31B C30B C4 106.4(15) . . ? C33 C31B C30B 125(2) . . ? C33 C31B C31B 42.1(13) . 18 ? C30B C31B C31B 101.6(12) . 18 ? N1 C21 C28 127.8(11) . . ? C27 C34 C36 116.6(11) . . ? C27 C34 N6 88(2) . . ? C36 C34 N6 155(2) . . ? C34 C36 C35 131.0(13) . . ? C34 C36 C36 114.3(12) . 11_455 ? C35 C36 C36 111.4(10) . 11_455 ? C34 C36 C36 113.0(8) . 19_575 ? C35 C36 C36 49.9(7) . 19_575 ? C36 C36 C36 90.000(3) 11_455 19_575 ? C15 C11 C6 115.3(10) . . ? O6A Zn1 O6A 158(5) . 2_575 ? O6A Zn1 O6B 158.8(5) . 2_575 ? O6A Zn1 O6B 32.6(18) 2_575 2_575 ? O6A Zn1 O6B 32.6(18) . 19_575 ? O6A Zn1 O6B 158.8(5) 2_575 19_575 ? O6B Zn1 O6B 129.2(4) 2_575 19_575 ? O6A Zn1 O6B 158.8(5) . 20 ? O6A Zn1 O6B 32.6(18) 2_575 20 ? O6B Zn1 O6B 41.6(4) 2_575 20 ? O6B Zn1 O6B 152.2(4) 19_575 20 ? O6A Zn1 O6B 32.6(18) . . ? O6A Zn1 O6B 158.8(5) 2_575 . ? O6B Zn1 O6B 152.2(4) 2_575 . ? O6B Zn1 O6B 41.6(4) 19_575 . ? O6B Zn1 O6B 129.2(4) 20 . ? O6A Zn1 O5B 74.9(6) . 19_575 ? O6A Zn1 O5B 109.0(4) 2_575 19_575 ? O6B Zn1 O5B 84.0(3) 2_575 19_575 ? O6B Zn1 O5B 49.9(2) 19_575 19_575 ? O6B Zn1 O5B 124.1(3) 20 19_575 ? O6B Zn1 O5B 91.2(3) . 19_575 ? O6A Zn1 O5B 109.0(3) . 2_575 ? O6A Zn1 O5B 74.9(6) 2_575 2_575 ? O6B Zn1 O5B 49.9(2) 2_575 2_575 ? O6B Zn1 O5B 84.0(3) 19_575 2_575 ? O6B Zn1 O5B 91.2(3) 20 2_575 ? O6B Zn1 O5B 124.1(3) . 2_575 ? O5B Zn1 O5B 34.8(4) 19_575 2_575 ? O6A Zn1 O5B 74.9(6) . . ? O6A Zn1 O5B 109.0(3) 2_575 . ? O6B Zn1 O5B 124.1(3) 2_575 . ? O6B Zn1 O5B 91.2(3) 19_575 . ? O6B Zn1 O5B 84.0(3) 20 . ? O6B Zn1 O5B 49.9(2) . . ? O5B Zn1 O5B 139.6(4) 19_575 . ? O5B Zn1 O5B 160.0(4) 2_575 . ? O6A Zn1 O5B 109.0(3) . 20 ? O6A Zn1 O5B 74.9(6) 2_575 20 ? O6B Zn1 O5B 91.2(3) 2_575 20 ? O6B Zn1 O5B 124.1(3) 19_575 20 ? O6B Zn1 O5B 49.9(2) 20 20 ? O6B Zn1 O5B 84.0(3) . 20 ? O5B Zn1 O5B 160.0(4) 19_575 20 ? O5B Zn1 O5B 139.6(4) 2_575 20 ? O5B Zn1 O5B 34.8(4) . 20 ? O6A Zn1 N2 79(2) . . ? O6A Zn1 N2 79(2) 2_575 . ? O6B Zn1 N2 103.92(18) 2_575 . ? O6B Zn1 N2 103.92(18) 19_575 . ? O6B Zn1 N2 103.92(18) 20 . ? O6B Zn1 N2 103.92(18) . . ? O5B Zn1 N2 100.0(2) 19_575 . ? O5B Zn1 N2 100.0(2) 2_575 . ? O5B Zn1 N2 100.0(2) . . ? O5B Zn1 N2 100.0(2) 20 . ? O6A Zn1 Zn3 101(2) . . ? O6A Zn1 Zn3 101(2) 2_575 . ? O6B Zn1 Zn3 76.08(18) 2_575 . ? O6B Zn1 Zn3 76.08(18) 19_575 . ? O6B Zn1 Zn3 76.08(18) 20 . ? O6B Zn1 Zn3 76.08(18) . . ? O5B Zn1 Zn3 80.0(2) 19_575 . ? O5B Zn1 Zn3 80.0(2) 2_575 . ? O5B Zn1 Zn3 80.0(2) . . ? O5B Zn1 Zn3 80.0(2) 20 . ? N2 Zn1 Zn3 180.000(1) . . ? O2 Zn3 O2 158.6(4) . 2_575 ? O2 Zn3 O1 87.49(5) . 2_575 ? O2 Zn3 O1 87.49(5) 2_575 2_575 ? O2 Zn3 O1 87.49(5) . . ? O2 Zn3 O1 87.49(5) 2_575 . ? O1 Zn3 O1 152.7(3) 2_575 . ? O2 Zn3 N1 100.68(18) . . ? O2 Zn3 N1 100.67(18) 2_575 . ? O1 Zn3 N1 103.66(16) 2_575 . ? O1 Zn3 N1 103.66(16) . . ? O2 Zn3 Zn1 79.32(18) . . ? O2 Zn3 Zn1 79.33(18) 2_575 . ? O1 Zn3 Zn1 76.34(16) 2_575 . ? O1 Zn3 Zn1 76.34(16) . . ? N1 Zn3 Zn1 180.000(2) . . ? O4 Zn2 O4 157.1(3) 14 . ? O4 Zn2 O3 85.3(3) 14 14 ? O4 Zn2 O3 89.8(3) . 14 ? O4 Zn2 O3 89.8(3) 14 . ? O4 Zn2 O3 85.3(3) . . ? O3 Zn2 O3 155.2(3) 14 . ? O4 Zn2 N3 101.44(16) 14 . ? O4 Zn2 N3 101.44(16) . . ? O3 Zn2 N3 102.38(16) 14 . ? O3 Zn2 N3 102.38(16) . . ? O4 Zn2 Zn2 78.56(16) 14 29 ? O4 Zn2 Zn2 78.56(16) . 29 ? O3 Zn2 Zn2 77.62(16) 14 29 ? O3 Zn2 Zn2 77.62(16) . 29 ? N3 Zn2 Zn2 180.0 . 29 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn2 O4 C1 O4 19.1(17) . . . 18 ? Zn2 O4 C1 C4 -173.0(5) . . . . ? Zn3 O1 C3 C3 106.1(5) . . . 20 ? C3 O1 C3 O5B -81.0(11) 20 . . . ? Zn3 O1 C3 O5B 25.1(13) . . . . ? C3 O1 C3 C6 88.3(9) 20 . . . ? Zn3 O1 C3 C6 -165.6(7) . . . . ? C3 O1 C3 O5B -38.1(7) 20 . . 20 ? Zn3 O1 C3 O5B 68.0(8) . . . 20 ? C3 O1 C3 C6 46.4(7) 20 . . 20 ? Zn3 O1 C3 C6 152.5(5) . . . 20 ? O4 C1 C4 C30A 28.0(10) 18 . . 18 ? O4 C1 C4 C30A -142.5(8) . . . 18 ? O4 C1 C4 C30A 142.5(8) 18 . . . ? O4 C1 C4 C30A -28.0(10) . . . . ? O4 C1 C4 C30B -27.8(11) 18 . . 18 ? O4 C1 C4 C30B 161.7(9) . . . 18 ? O4 C1 C4 C30B -161.7(9) 18 . . . ? O4 C1 C4 C30B 27.8(11) . . . . ? Zn2 O3 C5 O3 8.7(15) . . . 18 ? Zn2 O3 C5 C2 -176.0(6) . . . . ? C16A C2 C5 O3 21.3(13) . . . 18 ? C16A C2 C5 O3 154.5(10) 18 . . 18 ? C16B C2 C5 O3 -26.2(12) . . . 18 ? C16B C2 C5 O3 -158.0(8) 18 . . 18 ? C16A C2 C5 O3 -154.5(10) . . . . ? C16A C2 C5 O3 -21.3(13) 18 . . . ? C16B C2 C5 O3 158.0(8) . . . . ? C16B C2 C5 O3 26.2(12) 18 . . . ? C3 C3 C6 C6 0.0 20 . . 20 ? O5B C3 C6 C6 100.3(9) . . . 20 ? O1 C3 C6 C6 -70.0(7) . . . 20 ? O5B C3 C6 C6 48.1(7) 20 . . 20 ? C3 C3 C6 C11 -120.9(9) 20 . . . ? O5B C3 C6 C11 -20.6(16) . . . . ? O1 C3 C6 C11 169.1(8) . . . . ? O5B C3 C6 C11 -72.8(12) 20 . . . ? C6 C3 C6 C11 -120.9(9) 20 . . . ? C3 C3 C6 C12 53.8(11) 20 . . . ? O5B C3 C6 C12 154.1(10) . . . . ? O1 C3 C6 C12 -16.2(16) . . . . ? O5B C3 C6 C12 101.8(13) 20 . . . ? C6 C3 C6 C12 53.8(11) 20 . . . ? O5B C3 C6 C3 100.3(9) . . . 20 ? O1 C3 C6 C3 -70.0(7) . . . 20 ? O5B C3 C6 C3 48.1(7) 20 . . 20 ? C6 C3 C6 C3 0.0 20 . . 20 ? Zn3 O2 C7 C7 -102.9(4) . . . 19_575 ? C7 O2 C7 O6B 84.6(12) 19_575 . . . ? Zn3 O2 C7 O6B -18.3(14) . . . . ? C7 O2 C7 C8 -87.3(9) 19_575 . . . ? Zn3 O2 C7 C8 169.8(6) . . . . ? C7 O2 C7 O6B 34.6(7) 19_575 . . 19_575 ? Zn3 O2 C7 O6B -68.4(7) . . . 19_575 ? C7 O2 C7 C8 -47.0(6) 19_575 . . 19_575 ? Zn3 O2 C7 C8 -149.9(4) . . . 19_575 ? C7 C7 C8 C8 0.006(1) 19_575 . . 19_575 ? O6B C7 C8 C8 -103.4(8) . . . 19_575 ? O2 C7 C8 C8 70.1(8) . . . 19_575 ? O6B C7 C8 C8 -46.8(6) 19_575 . . 19_575 ? C7 C7 C8 C27 120.4(9) 19_575 . . . ? O6B C7 C8 C27 16.9(14) . . . . ? O2 C7 C8 C27 -169.5(8) . . . . ? O6B C7 C8 C27 73.6(11) 19_575 . . . ? C8 C7 C8 C27 120.4(9) 19_575 . . . ? C7 C7 C8 C26 -58.2(7) 19_575 . . . ? O6B C7 C8 C26 -161.7(8) . . . . ? O2 C7 C8 C26 11.9(13) . . . . ? O6B C7 C8 C26 -105.0(8) 19_575 . . . ? C8 C7 C8 C26 -58.2(7) 19_575 . . . ? O6B C7 C8 C7 -103.4(8) . . . 19_575 ? O2 C7 C8 C7 70.1(8) . . . 19_575 ? O6B C7 C8 C7 -46.8(6) 19_575 . . 19_575 ? C8 C7 C8 C7 -0.006(1) 19_575 . . 19_575 ? C10 N2 C10 C19 -0.004(5) 2_575 . . . ? Zn1 N2 C10 C19 180.000(3) . . . . ? C6 C6 C12 C14 -110.1(11) 20 . . . ? C11 C6 C12 C14 1.0(17) . . . . ? C3 C6 C12 C14 -173.4(10) . . . . ? C3 C6 C12 C14 -147.7(9) 20 . . . ? C11 C6 C12 C6 111.1(9) . . . 20 ? C3 C6 C12 C6 -63.3(13) . . . 20 ? C3 C6 C12 C6 -37.7(9) 20 . . 20 ? C6 C12 C14 C13 -6.6(16) . . . . ? C6 C12 C14 C13 -71.9(10) 20 . . . ? C6 C12 C14 C13 71.9(10) . . . 20 ? C6 C12 C14 C13 6.6(16) 20 . . 20 ? C13 C13 C14 C12 175.5(15) 8_565 . . . ? C15 C13 C14 C12 8.5(17) . . . . ? C13 C13 C14 C12 110.2(13) 20 . . . ? C13 C13 C14 C13 65.3(19) 8_565 . . 20 ? C15 C13 C14 C13 -101.8(12) . . . 20 ? C13 C13 C15 C11 -172.3(13) 8_565 . . . ? C14 C13 C15 C11 -6(2) . . . . ? C13 C13 C15 C11 -65.9(16) 20 . . . ? C13 C13 C15 N4 13(2) 8_565 . . . ? C14 C13 C15 N4 179.1(14) . . . . ? C13 C13 C15 N4 119.1(14) 20 . . . ? C19 C20 C19 C10 0.003(5) 2_575 . . . ? C20 C20 C19 C10 179.996(4) 17_575 . . . ? N2 C10 C19 C20 0.000(6) . . . . ? C28 C29 C28 C21 0.003(2) 2_575 . . . ? C29 C29 C28 C21 179.997(2) 17_576 . . . ? C8 C8 C26 C35 103.3(6) 19_575 . . . ? C27 C8 C26 C35 -4.8(14) . . . . ? C7 C8 C26 C35 173.5(7) . . . . ? C7 C8 C26 C35 147.3(6) 19_575 . . . ? C27 C8 C26 C8 -108.1(11) . . . 19_575 ? C7 C8 C26 C8 70.2(9) . . . 19_575 ? C7 C8 C26 C8 44.1(6) 19_575 . . 19_575 ? C8 C8 C27 C34 -84.0(11) 19_575 . . . ? C26 C8 C27 C34 -3.7(18) . . . . ? C7 C8 C27 C34 178.0(11) . . . . ? C7 C8 C27 C34 -148.0(11) 19_575 . . . ? N5 O7 N5 O8 -81(3) 19_565 . . . ? N5 O7 N5 C17A 92.0(17) 19_565 . . . ? C8 C26 C35 C36 -14.4(11) 19_575 . . 19_575 ? C8 C26 C35 C36 -72.4(9) . . . 19_575 ? C8 C26 C35 C36 72.4(9) 19_575 . . . ? C8 C26 C35 C36 14.4(11) . . . . ? C11 C15 N4 O10 50(3) . . . . ? C13 C15 N4 O10 -134(3) . . . . ? C11 C15 N4 O9 -161(2) . . . . ? C13 C15 N4 O9 15(3) . . . . ? C16A C2 C16A C17A 37(2) 18 . . . ? C16B C2 C16A C17A -89.2(17) . . . . ? C16B C2 C16A C17A -5(2) 18 . . . ? C5 C2 C16A C17A 176.0(11) . . . . ? C2 C16A C17A C18 9(2) . . . . ? C2 C16A C17A N5 -173.0(13) . . . . ? C17A C18 C17A C16A -50.0(15) 18 . . . ? C17B C18 C17A C16A -8.4(16) 18 . . . ? C17B C18 C17A C16A 75.1(14) . . . . ? C18 C18 C17A C16A 167.7(9) 19_565 . . . ? C17A C18 C17A N5 132.7(10) 18 . . . ? C17B C18 C17A N5 174.4(12) 18 . . . ? C17B C18 C17A N5 -102.1(16) . . . . ? C18 C18 C17A N5 -9.6(15) 19_565 . . . ? O7 N5 C17A C16A 155.6(14) . . . . ? O8 N5 C17A C16A -32(2) . . . . ? O7 N5 C17A C18 -27.0(19) . . . . ? O8 N5 C17A C18 146(2) . . . . ? C22A N3 C22A C23A 7.4(13) 14 . . . ? C22B N3 C22A C23A 80(2) 14 . . . ? C22B N3 C22A C23A -44.4(19) . . . . ? Zn2 N3 C22A C23A -172.5(13) . . . . ? C22B N3 C22A C22A 72.8(11) 14 . . 14 ? C22B N3 C22A C22A -51.9(9) . . . 14 ? Zn2 N3 C22A C22A -179.994(1) . . . 14 ? C23A C24 C23A C22A 4.8(8) 14 . . . ? C23B C24 C23A C22A -68.9(12) . . . . ? C23B C24 C23A C22A 53.9(12) 14 . . . ? C24 C24 C23A C22A -175.2(8) 11 . . . ? N3 C22A C23A C24 -14(2) . . . . ? C22A C22A C23A C24 -9.5(16) 14 . . . ? C30A C4 C30A C31A -61.9(15) 18 . . . ? C30B C4 C30A C31A -16.4(17) 18 . . . ? C30B C4 C30A C31A 71.8(13) . . . . ? C1 C4 C30A C31A 174.8(10) . . . . ? C4 C30A C31A C33 7.4(18) . . . . ? C31B C33 C31A C30A -8(3) 18 . . . ? C31B C33 C31A C30A -78(2) . . . . ? C33 C33 C31A C30A -177.7(10) 3_655 . . . ? C31A C33 C31A C30A 46(2) 18 . . . ? C3 C3 O5B O5B -0.002(3) 20 . . 20 ? O1 C3 O5B O5B 68.0(10) . . . 20 ? C6 C3 O5B O5B -100.8(10) . . . 20 ? C6 C3 O5B O5B -49.4(8) 20 . . 20 ? O1 C3 O5B C3 68.0(10) . . . 20 ? C6 C3 O5B C3 -100.8(10) . . . 20 ? O5B C3 O5B C3 0.002(2) 20 . . 20 ? C6 C3 O5B C3 -49.4(8) 20 . . 20 ? C3 C3 O5B O6B -133.9(4) 20 . . . ? O1 C3 O5B O6B -65.9(12) . . . . ? C6 C3 O5B O6B 125.3(10) . . . . ? O5B C3 O5B O6B -133.9(4) 20 . . . ? C6 C3 O5B O6B 176.7(7) 20 . . . ? C3 C3 O5B Zn1 -64.9(6) 20 . . . ? O1 C3 O5B Zn1 3.1(14) . . . . ? C6 C3 O5B Zn1 -165.7(8) . . . . ? O5B C3 O5B Zn1 -64.9(6) 20 . . . ? C6 C3 O5B Zn1 -114.3(9) 20 . . . ? C7 C7 O6B O6B -0.003(6) 19_575 . . 19_575 ? O2 C7 O6B O6B -71.1(11) . . . 19_575 ? C8 C7 O6B O6B 100.9(9) . . . 19_575 ? C8 C7 O6B O6B 53.5(7) 19_575 . . 19_575 ? C7 C7 O6B O5B 138.1(5) 19_575 . . . ? O2 C7 O6B O5B 67.0(14) . . . . ? C8 C7 O6B O5B -121.0(9) . . . . ? O6B C7 O6B O5B 138.1(5) 19_575 . . . ? C8 C7 O6B O5B -168.4(6) 19_575 . . . ? O2 C7 O6B C7 -71.1(11) . . . 19_575 ? C8 C7 O6B C7 100.9(9) . . . 19_575 ? O6B C7 O6B C7 0.003(5) 19_575 . . 19_575 ? C8 C7 O6B C7 53.5(7) 19_575 . . 19_575 ? C7 C7 O6B Zn1 57.3(5) 19_575 . . . ? O2 C7 O6B Zn1 -13.8(15) . . . . ? C8 C7 O6B Zn1 158.2(7) . . . . ? O6B C7 O6B Zn1 57.3(5) 19_575 . . . ? C8 C7 O6B Zn1 110.8(7) 19_575 . . . ? O5B O5B O6B C7 -99.0(8) 20 . . . ? C3 O5B O6B C7 1.8(11) . . . . ? C3 O5B O6B C7 -30.4(12) 20 . . . ? Zn1 O5B O6B C7 -116.1(8) . . . . ? O5B O5B O6B O6B 7.8(6) 20 . . 19_575 ? C3 O5B O6B O6B 108.6(7) . . . 19_575 ? C3 O5B O6B O6B 76.5(9) 20 . . 19_575 ? Zn1 O5B O6B O6B -9.3(4) . . . 19_575 ? O5B O5B O6B C7 -66.2(10) 20 . . 19_575 ? C3 O5B O6B C7 34.6(12) . . . 19_575 ? C3 O5B O6B C7 2.4(13) 20 . . 19_575 ? Zn1 O5B O6B C7 -83.4(8) . . . 19_575 ? O5B O5B O6B Zn1 17.1(3) 20 . . . ? C3 O5B O6B Zn1 117.9(7) . . . . ? C3 O5B O6B Zn1 85.8(8) 20 . . . ? C16A C2 C16B C17B 73.1(14) . . . . ? C16A C2 C16B C17B 0.6(18) 18 . . . ? C16B C2 C16B C17B -45.3(16) 18 . . . ? C5 C2 C16B C17B -178.6(9) . . . . ? C17A C18 C17B C16B -71.0(13) . . . . ? C17A C18 C17B C16B -2.8(16) 18 . . . ? C17B C18 C17B C16B 44.4(18) 18 . . . ? C18 C18 C17B C16B 173.6(9) 19_565 . . . ? C2 C16B C17B C18 -1.5(17) . . . . ? C22A N3 C22B C23B -50.6(14) 14 . . 14 ? C22A N3 C22B C23B 62.0(14) . . . 14 ? C22B N3 C22B C23B 13.9(9) 14 . . 14 ? Zn2 N3 C22B C23B -166.1(9) . . . 14 ? C23A C24 C23B C22B 81.5(11) . . . 14 ? C23A C24 C23B C22B -38.6(11) 14 . . 14 ? C23B C24 C23B C22B 9.8(6) 14 . . 14 ? C24 C24 C23B C22B -170.2(6) 11 . . 14 ? C30A C4 C30B C31B -21.1(19) 18 . . . ? C30A C4 C30B C31B -87.4(16) . . . . ? C30B C4 C30B C31B 35(2) 18 . . . ? C1 C4 C30B C31B 170.2(14) . . . . ? C31B C33 C31B C30B -66(3) 18 . . . ? C33 C33 C31B C30B 174.2(18) 3_655 . . . ? C31A C33 C31B C30B 63(2) . . . . ? C31A C33 C31B C30B -16(4) 18 . . . ? C33 C33 C31B C31B -120(2) 3_655 . . 18 ? C31A C33 C31B C31B 128.9(15) . . . 18 ? C31A C33 C31B C31B 50.5(14) 18 . . 18 ? C4 C30B C31B C33 20(3) . . . . ? C4 C30B C31B C31B -19.0(11) . . . 18 ? C21 N1 C21 C28 -0.003(2) 2_575 . . . ? Zn3 N1 C21 C28 180.000(1) . . . . ? C29 C28 C21 N1 0.000(2) . . . . ? C8 C27 C34 C36 -0.1(18) . . . . ? C8 C27 C34 N6 -175(2) . . . . ? C27 C34 C36 C35 14(2) . . . . ? N6 C34 C36 C35 -179(5) . . . . ? C27 C34 C36 C36 170.7(10) . . . 11_455 ? N6 C34 C36 C36 -22(6) . . . 11_455 ? C27 C34 C36 C36 69.7(13) . . . 19_575 ? N6 C34 C36 C36 -123(5) . . . 19_575 ? C26 C35 C36 C34 -21.3(19) . . . . ? C36 C35 C36 C34 86.9(17) 19_575 . . . ? C26 C35 C36 C36 -179.0(9) . . . 11_455 ? C36 C35 C36 C36 -70.8(12) 19_575 . . 11_455 ? C26 C35 C36 C36 -108.2(10) . . . 19_575 ? C13 C15 C11 C6 1(2) . . . . ? N4 C15 C11 C6 176.1(13) . . . . ? C6 C6 C11 C15 78.6(10) 20 . . . ? C3 C6 C11 C15 177.1(11) . . . . ? C12 C6 C11 C15 2.5(16) . . . . ? C3 C6 C11 C15 141.5(12) 20 . . . ? C7 O6B Zn1 O6A -116(3) . . . . ? O6B O6B Zn1 O6A -54(3) 19_575 . . . ? O5B O6B Zn1 O6A 133(3) . . . . ? C7 O6B Zn1 O6A -89(3) 19_575 . . . ? C7 O6B Zn1 O6A 106(7) . . . 2_575 ? O6B O6B Zn1 O6A 168(7) 19_575 . . 2_575 ? O5B O6B Zn1 O6A -5(7) . . . 2_575 ? C7 O6B Zn1 O6A 133(7) 19_575 . . 2_575 ? C7 O6B Zn1 O6B 22.1(7) . . . 2_575 ? O6B O6B Zn1 O6B 84.61(8) 19_575 . . 2_575 ? O5B O6B Zn1 O6B -88.6(3) . . . 2_575 ? C7 O6B Zn1 O6B 49.5(4) 19_575 . . 2_575 ? C7 O6B Zn1 O6B -62.5(7) . . . 19_575 ? O5B O6B Zn1 O6B -173.2(3) . . . 19_575 ? C7 O6B Zn1 O6B -35.1(5) 19_575 . . 19_575 ? C7 O6B Zn1 O6B 80.6(9) . . . 20 ? O6B O6B Zn1 O6B 143.1(4) 19_575 . . 20 ? O5B O6B Zn1 O6B -30.1(6) . . . 20 ? C7 O6B Zn1 O6B 108.0(5) 19_575 . . 20 ? C7 O6B Zn1 O5B -57.3(8) . . . 19_575 ? O6B O6B Zn1 O5B 5.2(2) 19_575 . . 19_575 ? O5B O6B Zn1 O5B -168.0(5) . . . 19_575 ? C7 O6B Zn1 O5B -29.9(5) 19_575 . . 19_575 ? C7 O6B Zn1 O5B -45.3(8) . . . 2_575 ? O6B O6B Zn1 O5B 17.2(2) 19_575 . . 2_575 ? O5B O6B Zn1 O5B -156.0(5) . . . 2_575 ? C7 O6B Zn1 O5B -17.9(5) 19_575 . . 2_575 ? C7 O6B Zn1 O5B 110.7(8) . . . . ? O6B O6B Zn1 O5B 173.2(3) 19_575 . . . ? C7 O6B Zn1 O5B 138.1(6) 19_575 . . . ? C7 O6B Zn1 O5B 103.3(8) . . . 20 ? O6B O6B Zn1 O5B 165.8(2) 19_575 . . 20 ? O5B O6B Zn1 O5B -7.42(17) . . . 20 ? C7 O6B Zn1 O5B 130.6(5) 19_575 . . 20 ? C7 O6B Zn1 N2 -157.9(7) . . . . ? O6B O6B Zn1 N2 -95.39(8) 19_575 . . . ? O5B O6B Zn1 N2 91.4(3) . . . . ? C7 O6B Zn1 N2 -130.5(4) 19_575 . . . ? C7 O6B Zn1 Zn3 22.1(7) . . . . ? O6B O6B Zn1 Zn3 84.61(8) 19_575 . . . ? O5B O6B Zn1 Zn3 -88.6(3) . . . . ? C7 O6B Zn1 Zn3 49.5(4) 19_575 . . . ? O5B O5B Zn1 O6A 169(2) 20 . . . ? C3 O5B Zn1 O6A -120(3) . . . . ? C3 O5B Zn1 O6A -152(2) 20 . . . ? O6B O5B Zn1 O6A -24(2) . . . . ? O5B O5B Zn1 O6A 11(3) 20 . . 2_575 ? C3 O5B Zn1 O6A 82(3) . . . 2_575 ? C3 O5B Zn1 O6A 50(3) 20 . . 2_575 ? O6B O5B Zn1 O6A 178(3) . . . 2_575 ? O5B O5B Zn1 O6B -21.3(2) 20 . . 2_575 ? C3 O5B Zn1 O6B 49.4(8) . . . 2_575 ? C3 O5B Zn1 O6B 17.5(6) 20 . . 2_575 ? O6B O5B Zn1 O6B 145.7(4) . . . 2_575 ? O5B O5B Zn1 O6B -162.5(2) 20 . . 19_575 ? C3 O5B Zn1 O6B -91.7(8) . . . 19_575 ? C3 O5B Zn1 O6B -123.6(5) 20 . . 19_575 ? O6B O5B Zn1 O6B 4.51(18) . . . 19_575 ? O5B O5B Zn1 O6B -10.0(2) 20 . . 20 ? C3 O5B Zn1 O6B 60.8(8) . . . 20 ? C3 O5B Zn1 O6B 28.9(5) 20 . . 20 ? O6B O5B Zn1 O6B 157.0(5) . . . 20 ? O5B O5B Zn1 O6B -167.0(3) 20 . . . ? C3 O5B Zn1 O6B -96.3(8) . . . . ? C3 O5B Zn1 O6B -128.1(6) 20 . . . ? O5B O5B Zn1 O5B -148.3(6) 20 . . 19_575 ? C3 O5B Zn1 O5B -77.5(10) . . . 19_575 ? C3 O5B Zn1 O5B -109.4(6) 20 . . 19_575 ? O6B O5B Zn1 O5B 18.7(7) . . . 19_575 ? O5B O5B Zn1 O5B -86.83(7) 20 . . 2_575 ? C3 O5B Zn1 O5B -16.1(7) . . . 2_575 ? C3 O5B Zn1 O5B -48.0(4) 20 . . 2_575 ? O6B O5B Zn1 O5B 80.2(3) . . . 2_575 ? C3 O5B Zn1 O5B 70.7(8) . . . 20 ? C3 O5B Zn1 O5B 38.9(5) 20 . . 20 ? O6B O5B Zn1 O5B 167.0(3) . . . 20 ? O5B O5B Zn1 N2 93.16(7) 20 . . . ? C3 O5B Zn1 N2 163.9(7) . . . . ? C3 O5B Zn1 N2 132.0(4) 20 . . . ? O6B O5B Zn1 N2 -99.9(3) . . . . ? O5B O5B Zn1 Zn3 -86.84(7) 20 . . . ? C3 O5B Zn1 Zn3 -16.1(7) . . . . ? C3 O5B Zn1 Zn3 -48.0(4) 20 . . . ? O6B O5B Zn1 Zn3 80.1(3) . . . . ? C10 N2 Zn1 O6A -90.000(4) . . . . ? C10 N2 Zn1 O6A 90.004(4) 2_575 . . . ? C10 N2 Zn1 O6A 89.995(4) . . . 2_575 ? C10 N2 Zn1 O6A -90.000(4) 2_575 . . 2_575 ? C10 N2 Zn1 O6B 111.44(19) . . . 2_575 ? C10 N2 Zn1 O6B -68.56(19) 2_575 . . 2_575 ? C10 N2 Zn1 O6B -111.44(19) . . . 19_575 ? C10 N2 Zn1 O6B 68.57(19) 2_575 . . 19_575 ? C10 N2 Zn1 O6B 68.56(19) . . . 20 ? C10 N2 Zn1 O6B -111.44(19) 2_575 . . 20 ? C10 N2 Zn1 O6B -68.56(19) . . . . ? C10 N2 Zn1 O6B 111.44(19) 2_575 . . . ? C10 N2 Zn1 O5B -162.3(2) . . . 19_575 ? C10 N2 Zn1 O5B 17.7(2) 2_575 . . 19_575 ? C10 N2 Zn1 O5B 162.3(2) . . . 2_575 ? C10 N2 Zn1 O5B -17.7(2) 2_575 . . 2_575 ? C10 N2 Zn1 O5B -17.7(2) . . . . ? C10 N2 Zn1 O5B 162.3(2) 2_575 . . . ? C10 N2 Zn1 O5B 17.7(2) . . . 20 ? C10 N2 Zn1 O5B -162.3(2) 2_575 . . 20 ? C10 N2 Zn1 Zn3 0(38) . . . . ? C10 N2 Zn1 Zn3 180(69) 2_575 . . . ? C7 O2 Zn3 O2 -24.2(6) 19_575 . . 2_575 ? C7 O2 Zn3 O2 24.2(6) . . . 2_575 ? C7 O2 Zn3 O1 52.4(6) 19_575 . . 2_575 ? C7 O2 Zn3 O1 100.7(6) . . . 2_575 ? C7 O2 Zn3 O1 -100.7(6) 19_575 . . . ? C7 O2 Zn3 O1 -52.4(6) . . . . ? C7 O2 Zn3 N1 155.8(6) 19_575 . . . ? C7 O2 Zn3 N1 -155.8(6) . . . . ? C7 O2 Zn3 Zn1 -24.2(6) 19_575 . . . ? C7 O2 Zn3 Zn1 24.2(6) . . . . ? C3 O1 Zn3 O2 53.4(6) . . . . ? C3 O1 Zn3 O2 105.8(6) 20 . . . ? C3 O1 Zn3 O2 -105.8(6) . . . 2_575 ? C3 O1 Zn3 O2 -53.4(6) 20 . . 2_575 ? C3 O1 Zn3 O1 -26.2(6) . . . 2_575 ? C3 O1 Zn3 O1 26.2(6) 20 . . 2_575 ? C3 O1 Zn3 N1 153.8(6) . . . . ? C3 O1 Zn3 N1 -153.8(6) 20 . . . ? C3 O1 Zn3 Zn1 -26.2(6) . . . . ? C3 O1 Zn3 Zn1 26.2(6) 20 . . . ? C21 N1 Zn3 O2 180.000(1) . . . . ? C21 N1 Zn3 O2 0.004(1) 2_575 . . . ? C21 N1 Zn3 O2 0.002(1) . . . 2_575 ? C21 N1 Zn3 O2 -179.994(1) 2_575 . . 2_575 ? C21 N1 Zn3 O1 -89.998(1) . . . 2_575 ? C21 N1 Zn3 O1 90.006(2) 2_575 . . 2_575 ? C21 N1 Zn3 O1 90.000(1) . . . . ? C21 N1 Zn3 O1 -89.996(1) 2_575 . . . ? C21 N1 Zn3 Zn1 0(38) . . . . ? C21 N1 Zn3 Zn1 0(36) 2_575 . . . ? O6A Zn1 Zn3 O2 0.0 . . . . ? O6A Zn1 Zn3 O2 180.0 2_575 . . . ? O6B Zn1 Zn3 O2 158.56(19) 2_575 . . . ? O6B Zn1 Zn3 O2 21.44(19) 19_575 . . . ? O6B Zn1 Zn3 O2 -158.56(19) 20 . . . ? O6B Zn1 Zn3 O2 -21.44(19) . . . . ? O5B Zn1 Zn3 O2 72.3(2) 19_575 . . . ? O5B Zn1 Zn3 O2 107.7(2) 2_575 . . . ? O5B Zn1 Zn3 O2 -72.3(2) . . . . ? O5B Zn1 Zn3 O2 -107.7(2) 20 . . . ? N2 Zn1 Zn3 O2 -90(100) . . . . ? O6A Zn1 Zn3 O2 180.0 . . . 2_575 ? O6A Zn1 Zn3 O2 0.0 2_575 . . 2_575 ? O6B Zn1 Zn3 O2 -21.44(19) 2_575 . . 2_575 ? O6B Zn1 Zn3 O2 -158.56(19) 19_575 . . 2_575 ? O6B Zn1 Zn3 O2 21.44(19) 20 . . 2_575 ? O6B Zn1 Zn3 O2 158.56(19) . . . 2_575 ? O5B Zn1 Zn3 O2 -107.7(2) 19_575 . . 2_575 ? O5B Zn1 Zn3 O2 -72.3(2) 2_575 . . 2_575 ? O5B Zn1 Zn3 O2 107.7(2) . . . 2_575 ? O5B Zn1 Zn3 O2 72.3(2) 20 . . 2_575 ? N2 Zn1 Zn3 O2 90(100) . . . 2_575 ? O6A Zn1 Zn3 O1 -90.002(1) . . . 2_575 ? O6A Zn1 Zn3 O1 90.002(1) 2_575 . . 2_575 ? O6B Zn1 Zn3 O1 68.56(19) 2_575 . . 2_575 ? O6B Zn1 Zn3 O1 -68.56(19) 19_575 . . 2_575 ? O6B Zn1 Zn3 O1 111.44(19) 20 . . 2_575 ? O6B Zn1 Zn3 O1 -111.44(19) . . . 2_575 ? O5B Zn1 Zn3 O1 -17.7(2) 19_575 . . 2_575 ? O5B Zn1 Zn3 O1 17.7(2) 2_575 . . 2_575 ? O5B Zn1 Zn3 O1 -162.3(2) . . . 2_575 ? O5B Zn1 Zn3 O1 162.3(2) 20 . . 2_575 ? N2 Zn1 Zn3 O1 180(100) . . . 2_575 ? O6A Zn1 Zn3 O1 90.0 . . . . ? O6A Zn1 Zn3 O1 -90.0 2_575 . . . ? O6B Zn1 Zn3 O1 -111.44(19) 2_575 . . . ? O6B Zn1 Zn3 O1 111.44(19) 19_575 . . . ? O6B Zn1 Zn3 O1 -68.56(19) 20 . . . ? O6B Zn1 Zn3 O1 68.56(19) . . . . ? O5B Zn1 Zn3 O1 162.3(2) 19_575 . . . ? O5B Zn1 Zn3 O1 -162.3(2) 2_575 . . . ? O5B Zn1 Zn3 O1 17.7(2) . . . . ? O5B Zn1 Zn3 O1 -17.7(2) 20 . . . ? N2 Zn1 Zn3 O1 0(100) . . . . ? O6A Zn1 Zn3 N1 0(100) . . . . ? O6A Zn1 Zn3 N1 0(53) 2_575 . . . ? O6B Zn1 Zn3 N1 0(36) 2_575 . . . ? O6B Zn1 Zn3 N1 0(100) 19_575 . . . ? O6B Zn1 Zn3 N1 0(84) 20 . . . ? O6B Zn1 Zn3 N1 0(100) . . . . ? O5B Zn1 Zn3 N1 0(100) 19_575 . . . ? O5B Zn1 Zn3 N1 0(100) 2_575 . . . ? O5B Zn1 Zn3 N1 0(100) . . . . ? O5B Zn1 Zn3 N1 0(100) 20 . . . ? N2 Zn1 Zn3 N1 0(100) . . . . ? C1 O4 Zn2 O4 -7.5(7) . . . 14 ? C1 O4 Zn2 O3 69.9(7) . . . 14 ? C1 O4 Zn2 O3 -85.8(7) . . . . ? C1 O4 Zn2 N3 172.5(7) . . . . ? C1 O4 Zn2 Zn2 -7.5(7) . . . 29 ? C5 O3 Zn2 O4 -82.2(7) . . . 14 ? C5 O3 Zn2 O4 75.4(7) . . . . ? C5 O3 Zn2 O3 -3.9(7) . . . 14 ? C5 O3 Zn2 N3 176.1(7) . . . . ? C5 O3 Zn2 Zn2 -3.9(7) . . . 29 ? C22A N3 Zn2 O4 177.6(11) 14 . . 14 ? C22A N3 Zn2 O4 -2.4(11) . . . 14 ? C22B N3 Zn2 O4 66.2(7) 14 . . 14 ? C22B N3 Zn2 O4 -113.8(7) . . . 14 ? C22A N3 Zn2 O4 -2.4(11) 14 . . . ? C22A N3 Zn2 O4 177.6(11) . . . . ? C22B N3 Zn2 O4 -113.8(7) 14 . . . ? C22B N3 Zn2 O4 66.2(7) . . . . ? C22A N3 Zn2 O3 89.9(10) 14 . . 14 ? C22A N3 Zn2 O3 -90.1(10) . . . 14 ? C22B N3 Zn2 O3 -21.5(7) 14 . . 14 ? C22B N3 Zn2 O3 158.5(7) . . . 14 ? C22A N3 Zn2 O3 -90.1(10) 14 . . . ? C22A N3 Zn2 O3 89.9(10) . . . . ? C22B N3 Zn2 O3 158.5(7) 14 . . . ? C22B N3 Zn2 O3 -21.5(7) . . . . ? C22A N3 Zn2 Zn2 52.3(19) 14 . . 29 ? C22A N3 Zn2 Zn2 -127.7(19) . . . 29 ? C22B N3 Zn2 Zn2 -59.1(18) 14 . . 29 ? C22B N3 Zn2 Zn2 120.9(18) . . . 29 ? _diffrn_measured_fraction_theta_max 0.810 _diffrn_reflns_theta_full 82.01 _diffrn_measured_fraction_theta_full 0.810 _refine_diff_density_max 3.301 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.221 _database_code_depnum_ccdc_archive 'CCDC 942881' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_BMOF-1-bpdc-NO2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'BMOF-1-bpdc-NO2 ' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H8 N6 O8 Zn2' _chemical_formula_weight 807.24 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 Orthorhombic _symmetry_space_group_name_H-M Cccm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z-1/2' _cell_length_a 21.3799(18) _cell_length_b 21.4597(18) _cell_length_c 27.944(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12821.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 7031 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.42 _exptl_crystal_description sheet _exptl_crystal_colour colourless _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 0.842 _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-II CCD' _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 40438 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.07 _reflns_number_total 5833 _reflns_number_gt 3286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Only nitrogen atom of the nitro group can be defined in the structure. The 4,4'-bpy is severely disordered, we cannot refine the ligand anisotropic and no hydrogen atom was added to the 4,4'-bpy ligand. SQUEEZE was applied to remove 9734 electrons that can belong to the disordered solvents and nitro groups. The ratio of max/min residual electron is little high due to the unresolved disordered nitro groups or solvent molecules that were not removed by the SQUEEZE. ; 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 -0.015 0.229 -0.005 9734 1530 ' ' _platon_squeeze_details ? _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^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5833 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 N1 N 0.0000 0.0000 0.12550(9) 0.0469(8) Uani 1 2 d S . . C5 C -0.22543(18) 0.22502(17) 0.25067(13) 0.1075(15) Uani 1 1 d . . . C7 C -0.14189(18) 0.17215(15) 0.28851(12) 0.1083(14) Uani 1 1 d . A . H7 H -0.1159 0.1679 0.3150 0.130 Uiso 1 1 calc R . . C6 C -0.1860(2) 0.21656(17) 0.28946(14) 0.1211(16) Uani 1 1 d . . . C8A C -0.0393(4) 0.0368(3) 0.1011(3) 0.0417(19) Uani 0.33 1 d P . . C9 C 0.0000 0.0000 0.02646(11) 0.0571(10) Uani 1 2 d S . . C8B C 0.0522(4) 0.0138(4) 0.1016(3) 0.042(2) Uani 0.33 1 d P . . N2A N -0.1739(4) 0.2803(7) 0.3352(4) 0.333(10) Uani 0.456(5) 1 d P A 2 N2B N -0.2815(7) 0.1735(4) 0.1663(4) 0.393(10) Uani 0.544(5) 1 d P A 1 C8C C 0.0124(5) 0.0532(3) 0.1007(2) 0.050(3) Uani 0.33 1 d P . . C10A C -0.0407(4) 0.0395(3) 0.0520(2) 0.0393(19) Uani 0.33 1 d P . . C10C C 0.0149(4) 0.0538(3) 0.0521(2) 0.039(2) Uani 0.33 1 d P . . C10B C -0.0538(4) -0.0139(2) 0.0520(2) 0.036(2) Uani 0.33 1 d P . . Zn1 Zn 0.0000 0.0000 0.198247(10) 0.03275(15) Uani 1 2 d S . . C1 C -0.08409(13) 0.08392(11) 0.25049(11) 0.0526(6) Uani 1 1 d . . . O1 O -0.07329(8) 0.05725(7) 0.21112(6) 0.0551(5) Uani 1 1 d . . . O2 O 0.05727(8) 0.07342(7) 0.21140(7) 0.0568(5) Uani 1 1 d . . . C2 C -0.13325(14) 0.13325(12) 0.25105(10) 0.0659(8) Uani 1 1 d . . . C3 C -0.17130(17) 0.14163(15) 0.21149(11) 0.1034(13) Uani 1 1 d . A . H3 H -0.1658 0.1163 0.1848 0.124 Uiso 1 1 calc R . . C4 C -0.21630(19) 0.18595(19) 0.21077(12) 0.1200(15) 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 N1 0.058(2) 0.0599(17) 0.0225(13) 0.000 0.000 0.032(2) C5 0.127(3) 0.128(3) 0.068(2) 0.008(2) 0.017(2) 0.090(3) C7 0.155(4) 0.111(3) 0.0586(19) -0.023(2) -0.022(2) 0.086(3) C6 0.151(4) 0.134(3) 0.078(2) -0.026(2) -0.013(3) 0.098(3) C8A 0.054(7) 0.032(5) 0.039(5) 0.009(3) 0.000(5) 0.001(4) C9 0.069(3) 0.079(2) 0.0225(17) 0.000 0.000 0.029(3) C8B 0.043(6) 0.055(6) 0.030(4) -0.001(3) -0.010(4) -0.021(4) N2A 0.107(8) 0.57(2) 0.317(14) -0.298(16) -0.014(8) 0.065(11) N2B 0.66(3) 0.166(8) 0.349(14) -0.040(8) -0.337(17) 0.105(12) C8C 0.101(10) 0.024(4) 0.024(4) 0.005(3) -0.018(4) -0.006(5) C10A 0.050(7) 0.028(3) 0.040(5) -0.005(3) 0.013(4) -0.001(4) C10C 0.047(7) 0.039(4) 0.032(4) 0.000(3) 0.009(3) -0.011(4) C10B 0.054(6) 0.016(4) 0.037(4) -0.002(2) 0.001(4) -0.003(3) Zn1 0.0406(3) 0.0390(2) 0.01859(19) 0.000 0.000 0.0008(2) C1 0.0546(19) 0.0540(13) 0.0494(15) 0.0008(16) -0.0023(19) 0.0135(12) O1 0.0577(13) 0.0631(10) 0.0446(10) -0.0104(9) -0.0085(10) 0.0191(9) O2 0.0666(14) 0.0549(10) 0.0489(10) 0.0042(8) -0.0124(10) -0.0232(9) C2 0.078(2) 0.0740(17) 0.0459(15) 0.0071(16) -0.0102(17) 0.0367(15) C3 0.121(3) 0.130(3) 0.059(2) -0.028(2) -0.016(2) 0.084(3) C4 0.141(4) 0.155(3) 0.063(2) -0.024(2) -0.019(2) 0.096(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 N1 C8B 1.334(8) . ? N1 C8B 1.334(8) 2 ? N1 C8A 1.341(8) 2 ? N1 C8A 1.341(8) . ? N1 C8C 1.361(7) 2 ? N1 C8C 1.361(7) . ? N1 Zn1 2.033(2) . ? C5 C6 1.385(5) . ? C5 C4 1.409(4) . ? C5 C5 1.501(6) 6_455 ? C7 C6 1.341(4) . ? C7 C2 1.352(4) . ? C7 H7 0.9300 . ? C6 N2A 1.890(10) . ? C8A C8B 1.121(10) 2 ? C8A C8C 1.162(11) . ? C8A C10A 1.373(10) . ? C8A C10B 1.777(10) . ? C8A C10C 1.830(10) . ? C8A C8C 2.015(9) 2 ? C8A C8B 2.019(11) . ? C9 C10B 1.387(8) . ? C9 C10B 1.387(8) 2 ? C9 C10C 1.395(7) 2 ? C9 C10C 1.395(7) . ? C9 C10A 1.408(7) 2 ? C9 C10A 1.408(7) . ? C9 C9 1.479(6) 9 ? C8B C8A 1.121(10) 2 ? C8B C8C 1.199(10) . ? C8B C10B 1.386(10) 2 ? C8B C10A 1.814(10) 2 ? C8B C10C 1.814(11) . ? C8B C8C 1.994(10) 2 ? N2B C4 1.886(11) . ? C8C C10C 1.361(9) . ? C8C C10A 1.798(11) . ? C8C C10B 1.828(12) 2 ? C8C C8B 1.994(10) 2 ? C8C C8A 2.015(9) 2 ? C10A C10B 1.179(9) . ? C10A C10C 1.227(10) . ? C10A C8B 1.814(10) 2 ? C10C C10B 1.194(10) 2 ? C10B C10C 1.194(10) 2 ? C10B C8B 1.386(10) 2 ? C10B C8C 1.828(12) 2 ? Zn1 O1 2.0233(16) . ? Zn1 O1 2.0234(16) 2 ? Zn1 O2 2.0289(15) . ? Zn1 O2 2.0290(15) 2 ? Zn1 Zn1 2.8925(6) 3 ? C1 O2 1.230(3) 3 ? C1 O1 1.261(3) . ? C1 C2 1.492(3) . ? O2 C1 1.230(3) 3 ? C2 C3 1.384(4) . ? C3 C4 1.353(4) . ? C3 H3 0.9300 . ? 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 C8B N1 C8B 119.9(6) . 2 ? C8B N1 C8A 49.5(4) . 2 ? C8B N1 C8A 98.0(5) 2 2 ? C8B N1 C8A 98.0(5) . . ? C8B N1 C8A 49.5(4) 2 . ? C8A N1 C8A 118.8(6) 2 . ? C8B N1 C8C 95.5(4) . 2 ? C8B N1 C8C 52.8(4) 2 2 ? C8A N1 C8C 50.9(5) 2 2 ? C8A N1 C8C 96.4(5) . 2 ? C8B N1 C8C 52.8(4) . . ? C8B N1 C8C 95.5(4) 2 . ? C8A N1 C8C 96.4(5) 2 . ? C8A N1 C8C 50.9(5) . . ? C8C N1 C8C 118.8(6) 2 . ? C8B N1 Zn1 120.0(3) . . ? C8B N1 Zn1 120.0(3) 2 . ? C8A N1 Zn1 120.6(3) 2 . ? C8A N1 Zn1 120.6(3) . . ? C8C N1 Zn1 120.6(3) 2 . ? C8C N1 Zn1 120.6(3) . . ? C6 C5 C4 117.2(3) . . ? C6 C5 C5 121.3(3) . 6_455 ? C4 C5 C5 121.5(3) . 6_455 ? C6 C7 C2 123.4(3) . . ? C6 C7 H7 118.3 . . ? C2 C7 H7 118.3 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 N2A 115.6(4) . . ? C5 C6 N2A 121.2(5) . . ? C8B C8A C8C 121.8(9) 2 . ? C8B C8A N1 64.9(6) 2 . ? C8C C8A N1 65.4(6) . . ? C8B C8A C10A 92.8(7) 2 . ? C8C C8A C10A 90.0(7) . . ? N1 C8A C10A 123.1(6) . . ? C8B C8A C10B 51.2(5) 2 . ? C8C C8A C10B 110.2(7) . . ? N1 C8A C10B 98.1(5) . . ? C10A C8A C10B 41.5(4) . . ? C8B C8A C10C 111.0(7) 2 . ? C8C C8A C10C 48.0(5) . . ? N1 C8A C10C 95.8(6) . . ? C10A C8A C10C 42.1(4) . . ? C10B C8A C10C 69.8(4) . . ? C8B C8A C8C 30.8(6) 2 2 ? C8C C8A C8C 91.0(7) . 2 ? N1 C8A C8C 42.2(3) . 2 ? C10A C8A C8C 92.3(5) . 2 ? C10B C8A C8C 57.2(4) . 2 ? C10C C8A C8C 90.4(5) . 2 ? C8B C8A C8B 90.0(7) 2 . ? C8C C8A C8B 31.8(5) . . ? N1 C8A C8B 40.9(3) . . ? C10A C8A C8B 92.2(6) . . ? C10B C8A C8B 91.4(5) . . ? C10C C8A C8B 56.0(4) . . ? C8C C8A C8B 59.3(4) 2 . ? C10B C9 C10B 117.9(6) . 2 ? C10B C9 C10C 50.8(4) . 2 ? C10B C9 C10C 95.9(4) 2 2 ? C10B C9 C10C 95.9(4) . . ? C10B C9 C10C 50.8(4) 2 . ? C10C C9 C10C 118.3(6) 2 . ? C10B C9 C10A 97.0(5) . 2 ? C10B C9 C10A 49.9(4) 2 2 ? C10C C9 C10A 51.9(4) 2 2 ? C10C C9 C10A 95.6(4) . 2 ? C10B C9 C10A 49.9(4) . . ? C10B C9 C10A 97.0(5) 2 . ? C10C C9 C10A 95.6(4) 2 . ? C10C C9 C10A 51.9(4) . . ? C10A C9 C10A 119.1(6) 2 . ? C10B C9 C9 121.0(3) . 9 ? C10B C9 C9 121.0(3) 2 9 ? C10C C9 C9 120.9(3) 2 9 ? C10C C9 C9 120.9(3) . 9 ? C10A C9 C9 120.4(3) 2 9 ? C10A C9 C9 120.4(3) . 9 ? C8A C8B C8C 120.6(9) 2 . ? C8A C8B N1 65.6(6) 2 . ? C8C C8B N1 64.8(6) . . ? C8A C8B C10B 89.7(7) 2 2 ? C8C C8B C10B 89.7(7) . 2 ? N1 C8B C10B 121.4(7) . 2 ? C8A C8B C10A 49.1(5) 2 2 ? C8C C8B C10A 109.4(7) . 2 ? N1 C8B C10A 97.4(5) . 2 ? C10B C8B C10A 40.6(4) 2 2 ? C8A C8B C10C 109.9(6) 2 . ? C8C C8B C10C 48.6(5) . . ? N1 C8B C10C 96.8(5) . . ? C10B C8B C10C 41.1(4) 2 . ? C10A C8B C10C 69.8(4) 2 . ? C8A C8B C8C 29.7(5) 2 2 ? C8C C8B C8C 90.9(6) . 2 ? N1 C8B C8C 42.8(3) . 2 ? C10B C8B C8C 90.3(5) 2 2 ? C10A C8B C8C 56.1(4) 2 2 ? C10C C8B C8C 91.5(5) . 2 ? C8A C8B C8A 89.9(7) 2 . ? C8C C8B C8A 30.7(5) . . ? N1 C8B C8A 41.1(3) . . ? C10B C8B C8A 90.9(6) 2 . ? C10A C8B C8A 91.0(5) 2 . ? C10C C8B C8A 56.8(4) . . ? C8C C8B C8A 60.3(4) 2 . ? C8A C8C C8B 117.6(8) . . ? C8A C8C C10C 92.7(7) . . ? C8B C8C C10C 90.0(8) . . ? C8A C8C N1 63.6(6) . . ? C8B C8C N1 62.4(5) . . ? C10C C8C N1 121.6(6) . . ? C8A C8C C10A 49.8(5) . . ? C8B C8C C10A 110.4(6) . . ? C10C C8C C10A 43.0(4) . . ? N1 C8C C10A 97.2(5) . . ? C8A C8C C10B 109.1(6) . 2 ? C8B C8C C10B 49.3(5) . 2 ? C10C C8C C10B 40.8(5) . 2 ? N1 C8C C10B 95.0(4) . 2 ? C10A C8C C10B 70.5(4) . 2 ? C8A C8C C8B 28.5(5) . 2 ? C8B C8C C8B 89.0(6) . 2 ? C10C C8C C8B 92.6(6) . 2 ? N1 C8C C8B 41.7(3) . 2 ? C10A C8C C8B 56.9(4) . 2 ? C10B C8C C8B 90.7(4) 2 2 ? C8A C8C C8A 89.0(7) . 2 ? C8B C8C C8A 28.6(4) . 2 ? C10C C8C C8A 90.2(6) . 2 ? N1 C8C C8A 41.4(3) . 2 ? C10A C8C C8A 91.6(4) . 2 ? C10B C8C C8A 54.8(4) 2 2 ? C8B C8C C8A 60.5(4) 2 2 ? C10B C10A C10C 118.3(8) . . ? C10B C10A C8A 87.9(7) . . ? C10C C10A C8A 89.3(7) . . ? C10B C10A C9 64.1(5) . . ? C10C C10A C9 63.5(5) . . ? C8A C10A C9 117.9(6) . . ? C10B C10A C8C 108.0(6) . . ? C10C C10A C8C 49.2(5) . . ? C8A C10A C8C 40.3(5) . . ? C9 C10A C8C 95.3(6) . . ? C10B C10A C8B 49.8(5) . 2 ? C10C C10A C8B 106.8(7) . 2 ? C8A C10A C8B 38.1(4) . 2 ? C9 C10A C8B 95.3(4) . 2 ? C8C C10A C8B 67.0(4) . 2 ? C10B C10C C10A 119.7(8) 2 . ? C10B C10C C8C 91.1(7) 2 . ? C10A C10C C8C 87.8(7) . . ? C10B C10C C9 64.2(5) 2 . ? C10A C10C C9 64.6(5) . . ? C8C C10C C9 119.7(6) . . ? C10B C10C C8B 49.8(5) 2 . ? C10A C10C C8B 108.0(6) . . ? C8C C10C C8B 41.4(5) . . ? C9 C10C C8B 95.8(5) . . ? C10B C10C C8A 107.4(6) 2 . ? C10A C10C C8A 48.6(5) . . ? C8C C10C C8A 39.3(5) . . ? C9 C10C C8A 94.3(5) . . ? C8B C10C C8A 67.3(4) . . ? C10A C10B C10C 122.0(9) . 2 ? C10A C10B C8B 89.6(6) . 2 ? C10C C10B C8B 89.1(7) 2 2 ? C10A C10B C9 66.0(5) . . ? C10C C10B C9 64.9(6) 2 . ? C8B C10B C9 119.6(7) 2 . ? C10A C10B C8A 50.5(5) . . ? C10C C10B C8A 108.5(7) 2 . ? C8B C10B C8A 39.1(4) 2 . ? C9 C10B C8A 97.0(5) . . ? C10A C10B C8C 109.5(7) . 2 ? C10C C10B C8C 48.1(5) 2 2 ? C8B C10B C8C 41.0(4) 2 2 ? C9 C10B C8C 94.7(6) . 2 ? C8A C10B C8C 67.9(4) . 2 ? O1 Zn1 O1 159.51(10) . 2 ? O1 Zn1 O2 87.92(8) . . ? O1 Zn1 O2 88.39(8) 2 . ? O1 Zn1 O2 88.39(8) . 2 ? O1 Zn1 O2 87.92(8) 2 2 ? O2 Zn1 O2 159.13(11) . 2 ? O1 Zn1 N1 100.24(5) . . ? O1 Zn1 N1 100.25(5) 2 . ? O2 Zn1 N1 100.43(5) . . ? O2 Zn1 N1 100.43(5) 2 . ? O1 Zn1 Zn1 79.76(5) . 3 ? O1 Zn1 Zn1 79.75(5) 2 3 ? O2 Zn1 Zn1 79.57(5) . 3 ? O2 Zn1 Zn1 79.57(5) 2 3 ? N1 Zn1 Zn1 180.0 . 3 ? O2 C1 O1 125.9(2) 3 . ? O2 C1 C2 116.7(2) 3 . ? O1 C1 C2 117.4(2) . . ? C1 O1 Zn1 124.92(16) . . ? C1 O2 Zn1 125.46(16) 3 . ? C7 C2 C3 117.3(3) . . ? C7 C2 C1 122.9(3) . . ? C3 C2 C1 119.9(2) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 N2B 115.8(4) . . ? C5 C4 N2B 120.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C7 C6 C5 -0.6(7) . . . . ? C2 C7 C6 N2A -161.5(6) . . . . ? C4 C5 C6 C7 -0.9(7) . . . . ? C5 C5 C6 C7 -179.2(4) 6_455 . . . ? C4 C5 C6 N2A 159.0(6) . . . . ? C5 C5 C6 N2A -19.3(9) 6_455 . . . ? C8B N1 C8A C8B 122.9(7) . . . 2 ? C8A N1 C8A C8B 75.0(5) 2 . . 2 ? C8C N1 C8A C8B 26.4(6) 2 . . 2 ? C8C N1 C8A C8B 148.6(7) . . . 2 ? Zn1 N1 C8A C8B -105.0(5) . . . 2 ? C8B N1 C8A C8C -25.8(6) . . . . ? C8B N1 C8A C8C -148.6(7) 2 . . . ? C8A N1 C8A C8C -73.7(5) 2 . . . ? C8C N1 C8A C8C -122.2(6) 2 . . . ? Zn1 N1 C8A C8C 106.3(5) . . . . ? C8B N1 C8A C10A 46.8(9) . . . . ? C8B N1 C8A C10A -76.0(9) 2 . . . ? C8A N1 C8A C10A -1.1(6) 2 . . . ? C8C N1 C8A C10A -49.6(8) 2 . . . ? C8C N1 C8A C10A 72.6(9) . . . . ? Zn1 N1 C8A C10A 178.9(6) . . . . ? C8B N1 C8A C10B 82.7(5) . . . . ? C8B N1 C8A C10B -40.1(5) 2 . . . ? C8A N1 C8A C10B 34.8(3) 2 . . . ? C8C N1 C8A C10B -13.7(5) 2 . . . ? C8C N1 C8A C10B 108.5(7) . . . . ? Zn1 N1 C8A C10B -145.2(3) . . . . ? C8B N1 C8A C10C 12.3(5) . . . . ? C8B N1 C8A C10C -110.5(6) 2 . . . ? C8A N1 C8A C10C -35.6(3) 2 . . . ? C8C N1 C8A C10C -84.1(5) 2 . . . ? C8C N1 C8A C10C 38.1(5) . . . . ? Zn1 N1 C8A C10C 144.4(3) . . . . ? C8B N1 C8A C8C 96.5(4) . . . 2 ? C8B N1 C8A C8C -26.4(6) 2 . . 2 ? C8A N1 C8A C8C 48.6(4) 2 . . 2 ? C8C N1 C8A C8C 122.2(6) . . . 2 ? Zn1 N1 C8A C8C -131.4(4) . . . 2 ? C8B N1 C8A C8B -122.9(7) 2 . . . ? C8A N1 C8A C8B -47.9(4) 2 . . . ? C8C N1 C8A C8B -96.5(4) 2 . . . ? C8C N1 C8A C8B 25.8(6) . . . . ? Zn1 N1 C8A C8B 132.1(4) . . . . ? C8B N1 C8B C8A -73.7(5) 2 . . 2 ? C8A N1 C8B C8A -121.3(7) . . . 2 ? C8C N1 C8B C8A -23.9(6) 2 . . 2 ? C8C N1 C8B C8A -146.3(7) . . . 2 ? Zn1 N1 C8B C8A 106.3(5) . . . 2 ? C8B N1 C8B C8C 72.6(5) 2 . . . ? C8A N1 C8B C8C 146.3(7) 2 . . . ? C8A N1 C8B C8C 25.1(6) . . . . ? C8C N1 C8B C8C 122.4(7) 2 . . . ? Zn1 N1 C8B C8C -107.4(5) . . . . ? C8B N1 C8B C10B -0.3(5) 2 . . 2 ? C8A N1 C8B C10B 73.4(8) 2 . . 2 ? C8A N1 C8B C10B -47.8(8) . . . 2 ? C8C N1 C8B C10B 49.5(7) 2 . . 2 ? C8C N1 C8B C10B -72.9(8) . . . 2 ? Zn1 N1 C8B C10B 179.7(5) . . . 2 ? C8B N1 C8B C10A -35.4(3) 2 . . 2 ? C8A N1 C8B C10A 38.3(5) 2 . . 2 ? C8A N1 C8B C10A -82.9(5) . . . 2 ? C8C N1 C8B C10A 14.4(5) 2 . . 2 ? C8C N1 C8B C10A -108.0(6) . . . 2 ? Zn1 N1 C8B C10A 144.6(3) . . . 2 ? C8B N1 C8B C10C 35.0(3) 2 . . . ? C8A N1 C8B C10C 108.8(6) 2 . . . ? C8A N1 C8B C10C -12.5(5) . . . . ? C8C N1 C8B C10C 84.8(5) 2 . . . ? C8C N1 C8B C10C -37.6(5) . . . . ? Zn1 N1 C8B C10C -145.0(3) . . . . ? C8B N1 C8B C8C -49.8(4) 2 . . 2 ? C8A N1 C8B C8C 23.9(6) 2 . . 2 ? C8A N1 C8B C8C -97.3(5) . . . 2 ? C8C N1 C8B C8C -122.4(7) . . . 2 ? Zn1 N1 C8B C8C 130.2(4) . . . 2 ? C8B N1 C8B C8A 47.5(4) 2 . . . ? C8A N1 C8B C8A 121.3(7) 2 . . . ? C8C N1 C8B C8A 97.3(5) 2 . . . ? C8C N1 C8B C8A -25.1(6) . . . . ? Zn1 N1 C8B C8A -132.5(4) . . . . ? C8B C8A C8B C8A 1.6(11) 2 . . 2 ? C8C C8A C8B C8A -177.6(10) . . . 2 ? N1 C8A C8B C8A 51.1(7) . . . 2 ? C10A C8A C8B C8A -91.2(7) . . . 2 ? C10B C8A C8B C8A -49.7(7) . . . 2 ? C10C C8A C8B C8A -114.0(6) . . . 2 ? C8C C8A C8B C8A 0.2(6) 2 . . 2 ? C8B C8A C8B C8C 179.2(10) 2 . . . ? N1 C8A C8B C8C -131.3(11) . . . . ? C10A C8A C8B C8C 86.4(9) . . . . ? C10B C8A C8B C8C 128.0(9) . . . . ? C10C C8A C8B C8C 63.6(8) . . . . ? C8C C8A C8B C8C 177.8(12) 2 . . . ? C8B C8A C8B N1 -49.5(6) 2 . . . ? C8C C8A C8B N1 131.3(11) . . . . ? C10A C8A C8B N1 -142.3(7) . . . . ? C10B C8A C8B N1 -100.8(5) . . . . ? C10C C8A C8B N1 -165.1(6) . . . . ? C8C C8A C8B N1 -50.9(3) 2 . . . ? C8B C8A C8B C10B 91.2(7) 2 . . 2 ? C8C C8A C8B C10B -88.0(10) . . . 2 ? N1 C8A C8B C10B 140.8(6) . . . 2 ? C10A C8A C8B C10B -1.6(6) . . . 2 ? C10B C8A C8B C10B 40.0(6) . . . 2 ? C10C C8A C8B C10B -24.4(5) . . . 2 ? C8C C8A C8B C10B 89.9(5) 2 . . 2 ? C8B C8A C8B C10A 50.7(7) 2 . . 2 ? C8C C8A C8B C10A -128.5(10) . . . 2 ? N1 C8A C8B C10A 100.2(5) . . . 2 ? C10A C8A C8B C10A -42.1(7) . . . 2 ? C10B C8A C8B C10A -0.6(5) . . . 2 ? C10C C8A C8B C10A -64.9(5) . . . 2 ? C8C C8A C8B C10A 49.3(4) 2 . . 2 ? C8B C8A C8B C10C 115.6(6) 2 . . . ? C8C C8A C8B C10C -63.6(8) . . . . ? N1 C8A C8B C10C 165.1(6) . . . . ? C10A C8A C8B C10C 22.8(5) . . . . ? C10B C8A C8B C10C 64.4(4) . . . . ? C8C C8A C8B C10C 114.2(5) 2 . . . ? C8B C8A C8B C8C 1.4(6) 2 . . 2 ? C8C C8A C8B C8C -177.8(12) . . . 2 ? N1 C8A C8B C8C 50.9(3) . . . 2 ? C10A C8A C8B C8C -91.4(6) . . . 2 ? C10B C8A C8B C8C -49.9(4) . . . 2 ? C10C C8A C8B C8C -114.2(5) . . . 2 ? C8B C8A C8C C8B -1.0(12) 2 . . . ? N1 C8A C8C C8B 32.7(7) . . . . ? C10A C8A C8C C8B -94.2(8) . . . . ? C10B C8A C8C C8B -57.1(9) . . . . ? C10C C8A C8C C8B -91.5(9) . . . . ? C8C C8A C8C C8B -1.9(10) 2 . . . ? C8B C8A C8C C10C 90.5(10) 2 . . . ? N1 C8A C8C C10C 124.2(6) . . . . ? C10A C8A C8C C10C -2.7(6) . . . . ? C10B C8A C8C C10C 34.4(7) . . . . ? C8C C8A C8C C10C 89.6(5) 2 . . . ? C8B C8A C8C C10C 91.5(9) . . . . ? C8B C8A C8C N1 -33.7(8) 2 . . . ? C10A C8A C8C N1 -126.9(5) . . . . ? C10B C8A C8C N1 -89.8(5) . . . . ? C10C C8A C8C N1 -124.2(6) . . . . ? C8C C8A C8C N1 -34.6(4) 2 . . . ? C8B C8A C8C N1 -32.7(7) . . . . ? C8B C8A C8C C10A 93.3(10) 2 . . . ? N1 C8A C8C C10A 126.9(5) . . . . ? C10B C8A C8C C10A 37.1(4) . . . . ? C10C C8A C8C C10A 2.7(6) . . . . ? C8C C8A C8C C10A 92.3(5) 2 . . . ? C8B C8A C8C C10A 94.2(8) . . . . ? C8B C8A C8C C10B 52.3(10) 2 . . 2 ? N1 C8A C8C C10B 86.0(5) . . . 2 ? C10A C8A C8C C10B -40.9(6) . . . 2 ? C10B C8A C8C C10B -3.8(8) . . . 2 ? C10C C8A C8C C10B -38.2(4) . . . 2 ? C8C C8A C8C C10B 51.4(6) 2 . . 2 ? C8B C8A C8C C10B 53.3(7) . . . 2 ? N1 C8A C8C C8B 33.7(8) . . . 2 ? C10A C8A C8C C8B -93.3(10) . . . 2 ? C10B C8A C8C C8B -56.1(8) . . . 2 ? C10C C8A C8C C8B -90.5(10) . . . 2 ? C8C C8A C8C C8B -0.9(7) 2 . . 2 ? C8B C8A C8C C8B 1.0(12) . . . 2 ? C8B C8A C8C C8A 0.4(11) 2 . . 2 ? N1 C8A C8C C8A 34.1(4) . . . 2 ? C10A C8A C8C C8A -92.9(5) . . . 2 ? C10B C8A C8C C8A -55.8(6) . . . 2 ? C10C C8A C8C C8A -90.1(6) . . . 2 ? C8C C8A C8C C8A -0.5(6) 2 . . 2 ? C8B C8A C8C C8A 1.3(6) . . . 2 ? C8A C8B C8C C8A 2.8(12) 2 . . . ? N1 C8B C8C C8A -33.1(7) . . . . ? C10B C8B C8C C8A 92.2(9) 2 . . . ? C10A C8B C8C C8A 56.0(10) 2 . . . ? C10C C8B C8C C8A 93.1(8) . . . . ? C8C C8B C8C C8A 1.9(10) 2 . . . ? C8A C8B C8C C10C -90.3(10) 2 . . . ? N1 C8B C8C C10C -126.2(6) . . . . ? C10B C8B C8C C10C -0.9(7) 2 . . . ? C10A C8B C8C C10C -37.1(9) 2 . . . ? C8C C8B C8C C10C -91.2(6) 2 . . . ? C8A C8B C8C C10C -93.1(8) . . . . ? C8A C8B C8C N1 35.9(8) 2 . . . ? C10B C8B C8C N1 125.3(5) 2 . . . ? C10A C8B C8C N1 89.2(6) 2 . . . ? C10C C8B C8C N1 126.2(6) . . . . ? C8C C8B C8C N1 35.0(4) 2 . . . ? C8A C8B C8C N1 33.1(7) . . . . ? C8A C8B C8C C10A -51.6(12) 2 . . . ? N1 C8B C8C C10A -87.5(7) . . . . ? C10B C8B C8C C10A 37.9(8) 2 . . . ? C10A C8B C8C C10A 1.7(10) 2 . . . ? C10C C8B C8C C10A 38.7(4) . . . . ? C8C C8B C8C C10A -52.5(8) 2 . . . ? C8A C8B C8C C10A -54.3(7) . . . . ? C8A C8B C8C C10B -89.4(9) 2 . . 2 ? N1 C8B C8C C10B -125.3(5) . . . 2 ? C10A C8B C8C C10B -36.2(5) 2 . . 2 ? C10C C8B C8C C10B 0.9(7) . . . 2 ? C8C C8B C8C C10B -90.3(5) 2 . . 2 ? C8A C8B C8C C10B -92.2(9) . . . 2 ? C8A C8B C8C C8B 2.3(11) 2 . . 2 ? N1 C8B C8C C8B -33.6(4) . . . 2 ? C10B C8B C8C C8B 91.8(5) 2 . . 2 ? C10A C8B C8C C8B 55.6(7) 2 . . 2 ? C10C C8B C8C C8B 92.6(6) . . . 2 ? C8C C8B C8C C8B 1.4(6) 2 . . 2 ? C8A C8B C8C C8B -0.5(6) . . . 2 ? N1 C8B C8C C8A -35.9(8) . . . 2 ? C10B C8B C8C C8A 89.4(9) 2 . . 2 ? C10A C8B C8C C8A 53.3(8) 2 . . 2 ? C10C C8B C8C C8A 90.3(10) . . . 2 ? C8C C8B C8C C8A -0.9(6) 2 . . 2 ? C8A C8B C8C C8A -2.8(12) . . . 2 ? C8B N1 C8C C8A 147.3(8) . . . . ? C8B N1 C8C C8A 23.4(6) 2 . . . ? C8A N1 C8C C8A 122.2(7) 2 . . . ? C8C N1 C8C C8A 73.6(5) 2 . . . ? Zn1 N1 C8C C8A -106.4(5) . . . . ? C8B N1 C8C C8B -123.8(7) 2 . . . ? C8A N1 C8C C8B -25.1(6) 2 . . . ? C8A N1 C8C C8B -147.3(8) . . . . ? C8C N1 C8C C8B -73.7(5) 2 . . . ? Zn1 N1 C8C C8B 106.3(5) . . . . ? C8B N1 C8C C10C 71.3(10) . . . . ? C8B N1 C8C C10C -52.5(9) 2 . . . ? C8A N1 C8C C10C 46.2(10) 2 . . . ? C8A N1 C8C C10C -75.9(9) . . . . ? C8C N1 C8C C10C -2.3(7) 2 . . . ? Zn1 N1 C8C C10C 177.7(7) . . . . ? C8B N1 C8C C10A 109.3(7) . . . . ? C8B N1 C8C C10A -14.5(5) 2 . . . ? C8A N1 C8C C10A 84.2(5) 2 . . . ? C8A N1 C8C C10A -38.0(5) . . . . ? C8C N1 C8C C10A 35.7(3) 2 . . . ? Zn1 N1 C8C C10A -144.4(3) . . . . ? C8B N1 C8C C10B 38.4(5) . . . 2 ? C8B N1 C8C C10B -85.5(5) 2 . . 2 ? C8A N1 C8C C10B 13.2(5) 2 . . 2 ? C8A N1 C8C C10B -108.9(6) . . . 2 ? C8C N1 C8C C10B -35.3(3) 2 . . 2 ? Zn1 N1 C8C C10B 144.7(3) . . . 2 ? C8B N1 C8C C8B 123.8(7) . . . 2 ? C8A N1 C8C C8B 98.7(5) 2 . . 2 ? C8A N1 C8C C8B -23.4(6) . . . 2 ? C8C N1 C8C C8B 50.2(4) 2 . . 2 ? Zn1 N1 C8C C8B -129.8(4) . . . 2 ? C8B N1 C8C C8A 25.1(6) . . . 2 ? C8B N1 C8C C8A -98.7(5) 2 . . 2 ? C8A N1 C8C C8A -122.2(7) . . . 2 ? C8C N1 C8C C8A -48.5(4) 2 . . 2 ? Zn1 N1 C8C C8A 131.5(4) . . . 2 ? C8B C8A C10A C10B -0.5(9) 2 . . . ? C8C C8A C10A C10B 121.4(8) . . . . ? N1 C8A C10A C10B 61.2(10) . . . . ? C10C C8A C10A C10B 118.3(8) . . . . ? C8C C8A C10A C10B 30.4(8) 2 . . . ? C8B C8A C10A C10B 89.7(7) . . . . ? C8B C8A C10A C10C -118.8(9) 2 . . . ? C8C C8A C10A C10C 3.0(7) . . . . ? N1 C8A C10A C10C -57.2(9) . . . . ? C10B C8A C10A C10C -118.3(8) . . . . ? C8C C8A C10A C10C -88.0(7) 2 . . . ? C8B C8A C10A C10C -28.6(6) . . . . ? C8B C8A C10A C9 -59.6(10) 2 . . . ? C8C C8A C10A C9 62.3(8) . . . . ? N1 C8A C10A C9 2.1(12) . . . . ? C10B C8A C10A C9 -59.1(6) . . . . ? C10C C8A C10A C9 59.2(7) . . . . ? C8C C8A C10A C9 -28.7(9) 2 . . . ? C8B C8A C10A C9 30.6(8) . . . . ? C8B C8A C10A C8C -121.8(9) 2 . . . ? N1 C8A C10A C8C -60.2(8) . . . . ? C10B C8A C10A C8C -121.4(8) . . . . ? C10C C8A C10A C8C -3.0(7) . . . . ? C8C C8A C10A C8C -91.0(7) 2 . . . ? C8B C8A C10A C8C -31.7(5) . . . . ? C8C C8A C10A C8B 121.8(9) . . . 2 ? N1 C8A C10A C8B 61.6(7) . . . 2 ? C10B C8A C10A C8B 0.5(9) . . . 2 ? C10C C8A C10A C8B 118.8(9) . . . 2 ? C8C C8A C10A C8B 30.8(6) 2 . . 2 ? C8B C8A C10A C8B 90.1(7) . . . 2 ? C10B C9 C10A C10B -120.9(7) 2 . . . ? C10C C9 C10A C10B -24.3(6) 2 . . . ? C10C C9 C10A C10B -146.2(7) . . . . ? C10A C9 C10A C10B -73.3(5) 2 . . . ? C9 C9 C10A C10B 106.7(5) 9 . . . ? C10B C9 C10A C10C 146.2(7) . . . . ? C10B C9 C10A C10C 25.2(5) 2 . . . ? C10C C9 C10A C10C 121.9(6) 2 . . . ? C10A C9 C10A C10C 72.8(5) 2 . . . ? C9 C9 C10A C10C -107.2(5) 9 . . . ? C10B C9 C10A C8A 72.4(8) . . . . ? C10B C9 C10A C8A -48.6(8) 2 . . . ? C10C C9 C10A C8A 48.1(8) 2 . . . ? C10C C9 C10A C8A -73.8(8) . . . . ? C10A C9 C10A C8A -1.0(6) 2 . . . ? C9 C9 C10A C8A 179.0(6) 9 . . . ? C10B C9 C10A C8C 107.4(6) . . . . ? C10B C9 C10A C8C -13.5(5) 2 . . . ? C10C C9 C10A C8C 83.1(5) 2 . . . ? C10C C9 C10A C8C -38.7(5) . . . . ? C10A C9 C10A C8C 34.1(3) 2 . . . ? C9 C9 C10A C8C -145.9(3) 9 . . . ? C10B C9 C10A C8B 40.1(5) . . . 2 ? C10B C9 C10A C8B -80.9(5) 2 . . 2 ? C10C C9 C10A C8B 15.8(5) 2 . . 2 ? C10C C9 C10A C8B -106.1(6) . . . 2 ? C10A C9 C10A C8B -33.3(3) 2 . . 2 ? C9 C9 C10A C8B 146.7(3) 9 . . 2 ? C8A C8C C10A C10B -63.8(9) . . . . ? C8B C8C C10A C10B 45.6(11) . . . . ? C10C C8C C10A C10B 112.2(9) . . . . ? N1 C8C C10A C10B -17.6(9) . . . . ? C10B C8C C10A C10B 75.2(7) 2 . . . ? C8B C8C C10A C10B -29.1(7) 2 . . . ? C8A C8C C10A C10B 23.6(9) 2 . . . ? C8A C8C C10A C10C -176.0(9) . . . . ? C8B C8C C10A C10C -66.6(9) . . . . ? N1 C8C C10A C10C -129.8(8) . . . . ? C10B C8C C10A C10C -37.0(5) 2 . . . ? C8B C8C C10A C10C -141.3(8) 2 . . . ? C8A C8C C10A C10C -88.6(7) 2 . . . ? C8B C8C C10A C8A 109.4(9) . . . . ? C10C C8C C10A C8A 176.0(9) . . . . ? N1 C8C C10A C8A 46.2(6) . . . . ? C10B C8C C10A C8A 139.0(7) 2 . . . ? C8B C8C C10A C8A 34.7(6) 2 . . . ? C8A C8C C10A C8A 87.4(7) 2 . . . ? C8A C8C C10A C9 -128.2(7) . . . . ? C8B C8C C10A C9 -18.8(9) . . . . ? C10C C8C C10A C9 47.7(6) . . . . ? N1 C8C C10A C9 -82.0(6) . . . . ? C10B C8C C10A C9 10.7(4) 2 . . . ? C8B C8C C10A C9 -93.5(5) 2 . . . ? C8A C8C C10A C9 -40.9(6) 2 . . . ? C8A C8C C10A C8B -34.7(6) . . . 2 ? C8B C8C C10A C8B 74.7(7) . . . 2 ? C10C C8C C10A C8B 141.3(8) . . . 2 ? N1 C8C C10A C8B 11.5(4) . . . 2 ? C10B C8C C10A C8B 104.3(5) 2 . . 2 ? C8A C8C C10A C8B 52.7(5) 2 . . 2 ? C10B C10A C10C C10B 0.2(11) . . . 2 ? C8A C10A C10C C10B 87.5(9) . . . 2 ? C9 C10A C10C C10B -34.5(7) . . . 2 ? C8C C10A C10C C10B 90.1(9) . . . 2 ? C8B C10A C10C C10B 53.1(9) 2 . . 2 ? C10B C10A C10C C8C -89.9(8) . . . . ? C8A C10A C10C C8C -2.6(6) . . . . ? C9 C10A C10C C8C -124.5(5) . . . . ? C8B C10A C10C C8C -37.0(7) 2 . . . ? C10B C10A C10C C9 34.7(7) . . . . ? C8A C10A C10C C9 122.0(5) . . . . ? C8C C10A C10C C9 124.5(5) . . . . ? C8B C10A C10C C9 87.6(5) 2 . . . ? C10B C10A C10C C8B -53.2(10) . . . . ? C8A C10A C10C C8B 34.1(6) . . . . ? C9 C10A C10C C8B -87.9(5) . . . . ? C8C C10A C10C C8B 36.7(4) . . . . ? C8B C10A C10C C8B -0.3(8) 2 . . . ? C10B C10A C10C C8A -87.3(8) . . . . ? C9 C10A C10C C8A -122.0(5) . . . . ? C8C C10A C10C C8A 2.6(6) . . . . ? C8B C10A C10C C8A -34.4(4) 2 . . . ? C8A C8C C10C C10B -116.6(7) . . . 2 ? C8B C8C C10C C10B 1.0(9) . . . 2 ? N1 C8C C10C C10B -56.1(11) . . . 2 ? C10A C8C C10C C10B -119.7(8) . . . 2 ? C8B C8C C10C C10B -88.0(7) 2 . . 2 ? C8A C8C C10C C10B -27.6(7) 2 . . 2 ? C8A C8C C10C C10A 3.1(7) . . . . ? C8B C8C C10C C10A 120.7(8) . . . . ? N1 C8C C10C C10A 63.6(10) . . . . ? C10B C8C C10C C10A 119.7(8) 2 . . . ? C8B C8C C10C C10A 31.6(6) 2 . . . ? C8A C8C C10C C10A 92.1(7) 2 . . . ? C8A C8C C10C C9 -55.9(9) . . . . ? C8B C8C C10C C9 61.7(10) . . . . ? N1 C8C C10C C9 4.6(14) . . . . ? C10A C8C C10C C9 -59.0(7) . . . . ? C10B C8C C10C C9 60.7(7) 2 . . . ? C8B C8C C10C C9 -27.3(10) 2 . . . ? C8A C8C C10C C9 33.1(10) 2 . . . ? C8A C8C C10C C8B -117.6(8) . . . . ? N1 C8C C10C C8B -57.1(7) . . . . ? C10A C8C C10C C8B -120.7(8) . . . . ? C10B C8C C10C C8B -1.0(9) 2 . . . ? C8B C8C C10C C8B -89.0(6) 2 . . . ? C8A C8C C10C C8B -28.6(4) 2 . . . ? C8B C8C C10C C8A 117.6(8) . . . . ? N1 C8C C10C C8A 60.5(8) . . . . ? C10A C8C C10C C8A -3.1(7) . . . . ? C10B C8C C10C C8A 116.6(7) 2 . . . ? C8B C8C C10C C8A 28.6(5) 2 . . . ? C8A C8C C10C C8A 89.0(7) 2 . . . ? C10B C9 C10C C10B 121.6(7) . . . 2 ? C10C C9 C10C C10B 73.3(5) 2 . . 2 ? C10A C9 C10C C10B 23.9(6) 2 . . 2 ? C10A C9 C10C C10B 146.9(7) . . . 2 ? C9 C9 C10C C10B -106.7(5) 9 . . 2 ? C10B C9 C10C C10A -25.4(5) . . . . ? C10B C9 C10C C10A -146.9(7) 2 . . . ? C10C C9 C10C C10A -73.6(4) 2 . . . ? C10A C9 C10C C10A -123.0(7) 2 . . . ? C9 C9 C10C C10A 106.4(4) 9 . . . ? C10B C9 C10C C8C 46.0(9) . . . . ? C10B C9 C10C C8C -75.5(9) 2 . . . ? C10C C9 C10C C8C -2.2(7) 2 . . . ? C10A C9 C10C C8C -51.6(9) 2 . . . ? C10A C9 C10C C8C 71.4(8) . . . . ? C9 C9 C10C C8C 177.8(7) 9 . . . ? C10B C9 C10C C8B 81.8(5) . . . . ? C10B C9 C10C C8B -39.7(5) 2 . . . ? C10C C9 C10C C8B 33.5(3) 2 . . . ? C10A C9 C10C C8B -15.8(5) 2 . . . ? C10A C9 C10C C8B 107.2(6) . . . . ? C9 C9 C10C C8B -146.5(3) 9 . . . ? C10B C9 C10C C8A 14.3(5) . . . . ? C10B C9 C10C C8A -107.3(6) 2 . . . ? C10C C9 C10C C8A -34.0(3) 2 . . . ? C10A C9 C10C C8A -83.3(5) 2 . . . ? C10A C9 C10C C8A 39.6(5) . . . . ? C9 C9 C10C C8A 146.0(3) 9 . . . ? C8A C8B C10C C10B -64.9(10) 2 . . 2 ? C8C C8B C10C C10B -178.7(11) . . . 2 ? N1 C8B C10C C10B -131.4(7) . . . 2 ? C10A C8B C10C C10B -36.0(6) 2 . . 2 ? C8C C8B C10C C10B -88.8(7) 2 . . 2 ? C8A C8B C10C C10B -141.2(8) . . . 2 ? C8A C8B C10C C10A 49.1(11) 2 . . . ? C8C C8B C10C C10A -64.6(9) . . . . ? N1 C8B C10C C10A -17.3(7) . . . . ? C10B C8B C10C C10A 114.1(9) 2 . . . ? C10A C8B C10C C10A 78.1(7) 2 . . . ? C8C C8B C10C C10A 25.3(7) 2 . . . ? C8A C8B C10C C10A -27.1(6) . . . . ? C8A C8B C10C C8C 113.7(10) 2 . . . ? N1 C8B C10C C8C 47.3(7) . . . . ? C10B C8B C10C C8C 178.7(11) 2 . . . ? C10A C8B C10C C8C 142.7(9) 2 . . . ? C8C C8B C10C C8C 89.9(7) 2 . . . ? C8A C8B C10C C8C 37.5(7) . . . . ? C8A C8B C10C C9 -16.0(10) 2 . . . ? C8C C8B C10C C9 -129.8(9) . . . . ? N1 C8B C10C C9 -82.5(5) . . . . ? C10B C8B C10C C9 48.9(6) 2 . . . ? C10A C8B C10C C9 13.0(4) 2 . . . ? C8C C8B C10C C9 -39.9(5) 2 . . . ? C8A C8B C10C C9 -92.3(5) . . . . ? C8A C8B C10C C8A 76.2(8) 2 . . . ? C8C C8B C10C C8A -37.5(7) . . . . ? N1 C8B C10C C8A 9.8(4) . . . . ? C10B C8B C10C C8A 141.2(8) 2 . . . ? C10A C8B C10C C8A 105.2(5) 2 . . . ? C8C C8B C10C C8A 52.4(4) 2 . . . ? C8B C8A C10C C10B -44.9(11) 2 . . 2 ? C8C C8A C10C C10B 69.5(8) . . . 2 ? N1 C8A C10C C10B 20.4(8) . . . 2 ? C10A C8A C10C C10B -114.6(8) . . . 2 ? C10B C8A C10C C10B -76.1(7) . . . 2 ? C8C C8A C10C C10B -21.5(8) 2 . . 2 ? C8B C8A C10C C10B 30.1(6) . . . 2 ? C8B C8A C10C C10A 69.7(10) 2 . . . ? C8C C8A C10C C10A -175.9(10) . . . . ? N1 C8A C10C C10A 135.0(7) . . . . ? C10B C8A C10C C10A 38.5(5) . . . . ? C8C C8A C10C C10A 93.1(7) 2 . . . ? C8B C8A C10C C10A 144.7(7) . . . . ? C8B C8A C10C C8C -114.4(11) 2 . . . ? N1 C8A C10C C8C -49.1(6) . . . . ? C10A C8A C10C C8C 175.9(10) . . . . ? C10B C8A C10C C8C -145.6(8) . . . . ? C8C C8A C10C C8C -91.0(7) 2 . . . ? C8B C8A C10C C8C -39.4(6) . . . . ? C8B C8A C10C C9 19.4(10) 2 . . . ? C8C C8A C10C C9 133.9(8) . . . . ? N1 C8A C10C C9 84.7(5) . . . . ? C10A C8A C10C C9 -50.2(5) . . . . ? C10B C8A C10C C9 -11.8(4) . . . . ? C8C C8A C10C C9 42.8(6) 2 . . . ? C8B C8A C10C C9 94.5(5) . . . . ? C8B C8A C10C C8B -75.0(8) 2 . . . ? C8C C8A C10C C8B 39.4(6) . . . . ? N1 C8A C10C C8B -9.7(4) . . . . ? C10A C8A C10C C8B -144.7(7) . . . . ? C10B C8A C10C C8B -106.2(5) . . . . ? C8C C8A C10C C8B -51.6(4) 2 . . . ? C10C C10A C10B C10C -0.1(11) . . . 2 ? C8A C10A C10B C10C -88.3(9) . . . 2 ? C9 C10A C10B C10C 34.3(8) . . . 2 ? C8C C10A C10B C10C -52.8(11) . . . 2 ? C8B C10A C10B C10C -88.7(9) 2 . . 2 ? C10C C10A C10B C8B 88.5(9) . . . 2 ? C8A C10A C10B C8B 0.4(8) . . . 2 ? C9 C10A C10B C8B 123.0(7) . . . 2 ? C8C C10A C10B C8B 35.8(9) . . . 2 ? C10C C10A C10B C9 -34.5(7) . . . . ? C8A C10A C10B C9 -122.6(6) . . . . ? C8C C10A C10B C9 -87.1(6) . . . . ? C8B C10A C10B C9 -123.0(7) 2 . . . ? C10C C10A C10B C8A 88.1(9) . . . . ? C9 C10A C10B C8A 122.6(6) . . . . ? C8C C10A C10B C8A 35.5(5) . . . . ? C8B C10A C10B C8A -0.4(8) 2 . . . ? C10C C10A C10B C8C 51.9(10) . . . 2 ? C8A C10A C10B C8C -36.2(8) . . . 2 ? C9 C10A C10B C8C 86.4(6) . . . 2 ? C8C C10A C10B C8C -0.7(10) . . . 2 ? C8B C10A C10B C8C -36.6(5) 2 . . 2 ? C10B C9 C10B C10A 74.5(5) 2 . . . ? C10C C9 C10B C10A 148.2(7) 2 . . . ? C10C C9 C10B C10A 26.1(6) . . . . ? C10A C9 C10B C10A 122.5(7) 2 . . . ? C9 C9 C10B C10A -105.5(5) 9 . . . ? C10B C9 C10B C10C -73.6(5) 2 . . 2 ? C10C C9 C10B C10C -122.0(6) . . . 2 ? C10A C9 C10B C10C -25.6(5) 2 . . 2 ? C10A C9 C10B C10C -148.2(7) . . . 2 ? C9 C9 C10B C10C 106.4(5) 9 . . 2 ? C10B C9 C10B C8B -0.3(5) 2 . . 2 ? C10C C9 C10B C8B 73.3(7) 2 . . 2 ? C10C C9 C10B C8B -48.7(7) . . . 2 ? C10A C9 C10B C8B 47.7(7) 2 . . 2 ? C10A C9 C10B C8B -74.8(7) . . . 2 ? C9 C9 C10B C8B 179.7(5) 9 . . 2 ? C10B C9 C10B C8A 33.6(3) 2 . . . ? C10C C9 C10B C8A 107.2(6) 2 . . . ? C10C C9 C10B C8A -14.8(5) . . . . ? C10A C9 C10B C8A 81.6(5) 2 . . . ? C10A C9 C10B C8A -40.9(5) . . . . ? C9 C9 C10B C8A -146.4(3) 9 . . . ? C10B C9 C10B C8C -34.7(3) 2 . . 2 ? C10C C9 C10B C8C 38.9(4) 2 . . 2 ? C10C C9 C10B C8C -83.1(4) . . . 2 ? C10A C9 C10B C8C 13.3(4) 2 . . 2 ? C10A C9 C10B C8C -109.3(6) . . . 2 ? C9 C9 C10B C8C 145.3(3) 9 . . 2 ? C8B C8A C10B C10A 179.4(12) 2 . . . ? C8C C8A C10B C10A -65.5(9) . . . . ? N1 C8A C10B C10A -132.2(9) . . . . ? C10C C8A C10B C10A -38.9(6) . . . . ? C8C C8A C10B C10A -143.1(9) 2 . . . ? C8B C8A C10B C10A -91.7(8) . . . . ? C8B C8A C10B C10C -63.9(9) 2 . . 2 ? C8C C8A C10B C10C 51.2(9) . . . 2 ? N1 C8A C10B C10C -15.5(8) . . . 2 ? C10A C8A C10B C10C 116.7(9) . . . 2 ? C10C C8A C10B C10C 77.7(7) . . . 2 ? C8C C8A C10B C10C -26.4(7) 2 . . 2 ? C8B C8A C10B C10C 25.0(7) . . . 2 ? C8C C8A C10B C8B 115.2(10) . . . 2 ? N1 C8A C10B C8B 48.4(7) . . . 2 ? C10A C8A C10B C8B -179.4(12) . . . 2 ? C10C C8A C10B C8B 141.7(10) . . . 2 ? C8C C8A C10B C8B 37.5(7) 2 . . 2 ? C8B C8A C10B C8B 88.9(8) . . . 2 ? C8B C8A C10B C9 -129.8(9) 2 . . . ? C8C C8A C10B C9 -14.6(7) . . . . ? N1 C8A C10B C9 -81.3(5) . . . . ? C10A C8A C10B C9 50.8(6) . . . . ? C10C C8A C10B C9 11.9(4) . . . . ? C8C C8A C10B C9 -92.3(6) 2 . . . ? C8B C8A C10B C9 -40.9(5) . . . . ? C8B C8A C10B C8C -37.5(7) 2 . . 2 ? C8C C8A C10B C8C 77.6(7) . . . 2 ? N1 C8A C10B C8C 10.9(4) . . . 2 ? C10A C8A C10B C8C 143.1(9) . . . 2 ? C10C C8A C10B C8C 104.2(6) . . . 2 ? C8B C8A C10B C8C 51.4(4) . . . 2 ? C8B N1 Zn1 O1 127.0(4) . . . . ? C8B N1 Zn1 O1 -53.0(4) 2 . . . ? C8A N1 Zn1 O1 -174.9(5) 2 . . . ? C8A N1 Zn1 O1 5.1(5) . . . . ? C8C N1 Zn1 O1 -115.0(5) 2 . . . ? C8C N1 Zn1 O1 65.0(5) . . . . ? C8B N1 Zn1 O1 -53.0(4) . . . 2 ? C8B N1 Zn1 O1 127.0(4) 2 . . 2 ? C8A N1 Zn1 O1 5.1(5) 2 . . 2 ? C8A N1 Zn1 O1 -174.9(5) . . . 2 ? C8C N1 Zn1 O1 65.0(5) 2 . . 2 ? C8C N1 Zn1 O1 -115.0(5) . . . 2 ? C8B N1 Zn1 O2 37.3(4) . . . . ? C8B N1 Zn1 O2 -142.7(4) 2 . . . ? C8A N1 Zn1 O2 95.3(5) 2 . . . ? C8A N1 Zn1 O2 -84.7(5) . . . . ? C8C N1 Zn1 O2 155.3(5) 2 . . . ? C8C N1 Zn1 O2 -24.7(5) . . . . ? C8B N1 Zn1 O2 -142.7(4) . . . 2 ? C8B N1 Zn1 O2 37.3(4) 2 . . 2 ? C8A N1 Zn1 O2 -84.7(5) 2 . . 2 ? C8A N1 Zn1 O2 95.3(5) . . . 2 ? C8C N1 Zn1 O2 -24.7(5) 2 . . 2 ? C8C N1 Zn1 O2 155.3(5) . . . 2 ? C8B N1 Zn1 Zn1 -141.6(4) . . . 3 ? C8B N1 Zn1 Zn1 38.4(4) 2 . . 3 ? C8A N1 Zn1 Zn1 -83.6(5) 2 . . 3 ? C8A N1 Zn1 Zn1 96.4(5) . . . 3 ? C8C N1 Zn1 Zn1 -23.6(5) 2 . . 3 ? C8C N1 Zn1 Zn1 156.4(5) . . . 3 ? O2 C1 O1 Zn1 -10.1(4) 3 . . . ? C2 C1 O1 Zn1 169.12(18) . . . . ? O1 Zn1 O1 C1 17.32(19) 2 . . . ? O2 Zn1 O1 C1 -62.5(2) . . . . ? O2 Zn1 O1 C1 97.0(2) 2 . . . ? N1 Zn1 O1 C1 -162.68(19) . . . . ? Zn1 Zn1 O1 C1 17.32(19) 3 . . . ? O1 Zn1 O2 C1 98.3(2) . . . 3 ? O1 Zn1 O2 C1 -61.6(2) 2 . . 3 ? O2 Zn1 O2 C1 18.3(2) 2 . . 3 ? N1 Zn1 O2 C1 -161.7(2) . . . 3 ? Zn1 Zn1 O2 C1 18.3(2) 3 . . 3 ? C6 C7 C2 C3 1.8(6) . . . . ? C6 C7 C2 C1 -179.8(3) . . . . ? O2 C1 C2 C7 10.7(4) 3 . . . ? O1 C1 C2 C7 -168.6(3) . . . . ? O2 C1 C2 C3 -171.0(3) 3 . . . ? O1 C1 C2 C3 9.7(4) . . . . ? C7 C2 C3 C4 -1.6(6) . . . . ? C1 C2 C3 C4 -179.9(3) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C2 C3 C4 N2B -158.6(6) . . . . ? C6 C5 C4 C3 1.1(7) . . . . ? C5 C5 C4 C3 179.4(4) 6_455 . . . ? C6 C5 C4 N2B 158.8(6) . . . . ? C5 C5 C4 N2B -22.9(8) 6_455 . . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 0.534 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.045 _database_code_depnum_ccdc_archive 'CCDC 942882' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_DMOF-1-bpdc-NO2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DMOF-1-bpdc-NO2 _chemical_melting_point ? _chemical_formula_moiety 'C36 N2 O8 Zn2' _chemical_formula_sum 'C36 H0 N2 O8 Zn2' _chemical_formula_weight 719.12 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' 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' 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 I4/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' 'y, -x, z' 'x, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, z' 'y, x, -z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1/2, y+1/2, -z+1' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' '-x, -y, -z' 'y, -x, -z' '-y, x, -z' '-x, y, z-1/2' 'x, -y, z-1/2' 'x, y, -z' '-y, -x, z-1/2' 'y, x, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 21.355(2) _cell_length_b 21.355(2) _cell_length_c 19.211(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8760.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 2769 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 22.12 _exptl_crystal_description square _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8912 _exptl_absorpt_correction_T_max 0.9671 _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-II CCD' _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 14536 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.86 _reflns_number_total 2500 _reflns_number_gt 1376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. No hydrogen atom was added to the dabco ligand due to the severely disordered. The nitro functional group was disordered and cannot be located in the structure, thus error Alert A and B or C4 for high Ueq. SQUEEZE was applied to the structure to find 892 electrons belong to disordered nitro groups, EtOAc, and DMF molecules. The ADP of the biphenyl rings were quite high due to the quality of the structure. It is somewhat typical for MOFs structure after the structure is refined anisotrpoically. ; 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 -0.023 0.299 -0.011 6467 892 ' ' _platon_squeeze_details ? _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^)+(0.1523P)^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 2500 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.2398 _refine_ls_wR_factor_gt 0.2214 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 C1 C 0.0734(3) 0.0941(3) 0.0000 0.0686(19) Uani 1 2 d S . . C2 C 0.1165(4) 0.1482(4) 0.0000 0.122(3) Uani 1 2 d S . . C5 C 0.1997(7) 0.2517(6) 0.0000 0.228(7) Uani 1 2 d S . . C3 C 0.1385(5) 0.1742(4) 0.0582(3) 0.233(5) Uani 1 1 d . . . C4 C 0.1792(6) 0.2230(5) 0.0576(3) 0.293(7) Uani 1 1 d . . . C6 C 0.0657(4) 0.0112(4) 0.2089(5) 0.066(2) Uiso 0.50 1 d P . . C7 C 0.0537(5) -0.0362(5) 0.2096(5) 0.074(3) Uiso 0.50 1 d P . . Zn1 Zn 0.0000 0.0000 0.07575(3) 0.0338(3) Uani 1 4 d S . . N1 N 0.0000 0.0000 0.1812(3) 0.0346(12) Uani 1 4 d S . . O1 O 0.05621(16) 0.07394(15) 0.05748(18) 0.0888(12) 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 C1 0.092(4) 0.081(4) 0.033(3) 0.000 0.000 -0.047(4) C2 0.169(7) 0.158(7) 0.040(3) 0.000 0.000 -0.130(6) C5 0.340(14) 0.295(12) 0.048(4) 0.000 0.000 -0.278(11) C3 0.356(11) 0.290(10) 0.052(3) -0.033(4) 0.034(4) -0.279(9) C4 0.454(14) 0.369(12) 0.056(3) -0.036(5) 0.046(6) -0.362(12) Zn1 0.0349(4) 0.0349(4) 0.0317(5) 0.000 0.000 0.000 N1 0.0318(17) 0.0318(17) 0.040(3) 0.000 0.000 0.000 O1 0.122(3) 0.092(2) 0.0528(17) -0.0175(15) 0.0250(16) -0.071(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 C1 O1 1.241(4) 22 ? C1 O1 1.241(4) . ? C1 C2 1.477(8) . ? C2 C3 1.333(7) . ? C2 C3 1.333(7) 22 ? C5 C4 1.338(8) 22 ? C5 C4 1.338(8) . ? C5 C5 1.467(15) 31 ? C3 C4 1.357(9) . ? C6 C7 1.044(10) . ? C6 C7 1.106(11) 2 ? C6 N1 1.520(10) . ? C6 C6 1.650(19) 4 ? C6 C7 1.675(15) 4 ? C6 C6 2.014(13) 2 ? C6 C6 2.014(13) 3 ? C7 C6 1.106(11) 3 ? C7 N1 1.487(10) . ? C7 C7 1.64(2) 8 ? C7 C6 1.675(15) 4 ? C7 C7 1.957(15) 3 ? C7 C7 1.957(15) 2 ? Zn1 O1 2.014(3) 6 ? Zn1 O1 2.014(3) 3 ? Zn1 O1 2.014(3) . ? Zn1 O1 2.014(3) 2 ? Zn1 N1 2.026(5) . ? Zn1 Zn1 2.9105(13) 17 ? N1 C7 1.487(10) 3 ? N1 C7 1.487(10) 6 ? N1 C7 1.487(10) 2 ? N1 C6 1.520(10) 3 ? N1 C6 1.520(10) 6 ? N1 C6 1.520(10) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O1 125.7(5) 22 . ? O1 C1 C2 117.1(3) 22 . ? O1 C1 C2 117.1(3) . . ? C3 C2 C3 113.8(7) . 22 ? C3 C2 C1 123.1(3) . . ? C3 C2 C1 123.1(3) 22 . ? C4 C5 C4 111.5(8) 22 . ? C4 C5 C5 123.7(4) 22 31 ? C4 C5 C5 123.7(4) . 31 ? C2 C3 C4 122.6(6) . . ? C5 C4 C3 124.6(7) . . ? C7 C6 C7 131.0(14) . 2 ? C7 C6 N1 68.0(7) . . ? C7 C6 N1 66.8(7) 2 . ? C7 C6 C6 73.0(9) . 4 ? C7 C6 C6 103.1(10) 2 4 ? N1 C6 C6 106.8(4) . 4 ? C7 C6 C7 105.1(10) . 4 ? C7 C6 C7 68.9(10) 2 4 ? N1 C6 C7 103.7(7) . 4 ? C6 C6 C7 36.6(4) 4 4 ? C7 C6 C6 111.1(7) . 2 ? C7 C6 C6 19.9(7) 2 2 ? N1 C6 C6 48.52(14) . 2 ? C6 C6 C6 99.6(3) 4 2 ? C7 C6 C6 72.0(6) 4 2 ? C7 C6 C6 21.1(7) . 3 ? C7 C6 C6 109.9(7) 2 3 ? N1 C6 C6 48.52(14) . 3 ? C6 C6 C6 76.3(6) 4 3 ? C7 C6 C6 99.9(5) 4 3 ? C6 C6 C6 90.002(1) 2 3 ? C6 C7 C6 139.0(14) . 3 ? C6 C7 N1 71.4(8) . . ? C6 C7 N1 70.0(7) 3 . ? C6 C7 C7 106.8(11) . 8 ? C6 C7 C7 72.1(9) 3 8 ? N1 C7 C7 106.8(5) . 8 ? C6 C7 C6 70.4(10) . 4 ? C6 C7 C6 108.6(9) 3 4 ? N1 C7 C6 107.2(8) . 4 ? C7 C7 C6 39.0(5) 8 4 ? C6 C7 C7 115.3(8) . 3 ? C6 C7 C7 23.7(7) 3 3 ? N1 C7 C7 48.86(15) . 3 ? C7 C7 C7 74.5(7) 8 3 ? C6 C7 C7 102.2(4) 4 3 ? C6 C7 C7 25.3(8) . 2 ? C6 C7 C7 113.7(7) 3 2 ? N1 C7 C7 48.86(15) . 2 ? C7 C7 C7 100.4(3) 8 2 ? C6 C7 C7 73.5(6) 4 2 ? C7 C7 C7 90.001(1) 3 2 ? O1 Zn1 O1 88.26(3) 6 3 ? O1 Zn1 O1 159.9(2) 6 . ? O1 Zn1 O1 88.26(3) 3 . ? O1 Zn1 O1 88.26(3) 6 2 ? O1 Zn1 O1 159.9(2) 3 2 ? O1 Zn1 O1 88.26(3) . 2 ? O1 Zn1 N1 100.04(10) 6 . ? O1 Zn1 N1 100.04(10) 3 . ? O1 Zn1 N1 100.04(10) . . ? O1 Zn1 N1 100.04(10) 2 . ? O1 Zn1 Zn1 79.96(10) 6 17 ? O1 Zn1 Zn1 79.96(10) 3 17 ? O1 Zn1 Zn1 79.96(10) . 17 ? O1 Zn1 Zn1 79.96(10) 2 17 ? N1 Zn1 Zn1 180.0 . 17 ? C7 N1 C7 82.3(3) . 3 ? C7 N1 C7 137.0(9) . 6 ? C7 N1 C7 82.3(3) 3 6 ? C7 N1 C7 82.3(3) . 2 ? C7 N1 C7 137.0(9) 3 2 ? C7 N1 C7 82.3(3) 6 2 ? C7 N1 C6 40.6(4) . . ? C7 N1 C6 118.2(5) 3 . ? C7 N1 C6 120.2(5) 6 . ? C7 N1 C6 43.2(4) 2 . ? C7 N1 C6 43.2(4) . 3 ? C7 N1 C6 40.6(4) 3 3 ? C7 N1 C6 118.2(5) 6 3 ? C7 N1 C6 120.2(5) 2 3 ? C6 N1 C6 83.0(3) . 3 ? C7 N1 C6 120.2(5) . 6 ? C7 N1 C6 43.2(4) 3 6 ? C7 N1 C6 40.6(4) 6 6 ? C7 N1 C6 118.2(5) 2 6 ? C6 N1 C6 139.0(8) . 6 ? C6 N1 C6 83.0(3) 3 6 ? C7 N1 C6 118.2(5) . 2 ? C7 N1 C6 120.2(5) 3 2 ? C7 N1 C6 43.2(4) 6 2 ? C7 N1 C6 40.6(4) 2 2 ? C6 N1 C6 83.0(3) . 2 ? C6 N1 C6 139.0(8) 3 2 ? C6 N1 C6 83.0(3) 6 2 ? C7 N1 Zn1 111.5(4) . . ? C7 N1 Zn1 111.5(4) 3 . ? C7 N1 Zn1 111.5(4) 6 . ? C7 N1 Zn1 111.5(4) 2 . ? C6 N1 Zn1 110.5(4) . . ? C6 N1 Zn1 110.5(4) 3 . ? C6 N1 Zn1 110.5(4) 6 . ? C6 N1 Zn1 110.5(4) 2 . ? C1 O1 Zn1 127.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -180.0(8) 22 . . . ? O1 C1 C2 C3 2.0(13) . . . . ? O1 C1 C2 C3 -2.0(13) 22 . . 22 ? O1 C1 C2 C3 180.0(8) . . . 22 ? C3 C2 C3 C4 0(2) 22 . . . ? C1 C2 C3 C4 178.4(11) . . . . ? C4 C5 C4 C3 -5(3) 22 . . . ? C5 C5 C4 C3 -173.9(10) 31 . . . ? C2 C3 C4 C5 3(2) . . . . ? C7 C6 C7 C6 3(4) 2 . . 3 ? N1 C6 C7 C6 -21(2) . . . 3 ? C6 C6 C7 C6 96(2) 4 . . 3 ? C7 C6 C7 C6 78(2) 4 . . 3 ? C6 C6 C7 C6 2(2) 2 . . 3 ? C7 C6 C7 N1 24.0(17) 2 . . . ? C6 C6 C7 N1 116.8(5) 4 . . . ? C7 C6 C7 N1 98.9(8) 4 . . . ? C6 C6 C7 N1 22.8(5) 2 . . . ? C6 C6 C7 N1 21(2) 3 . . . ? C7 C6 C7 C7 -78.6(19) 2 . . 8 ? N1 C6 C7 C7 -102.6(6) . . . 8 ? C6 C6 C7 C7 14.2(5) 4 . . 8 ? C7 C6 C7 C7 -3.6(12) 4 . . 8 ? C6 C6 C7 C7 -79.8(7) 2 . . 8 ? C6 C6 C7 C7 -81.9(19) 3 . . 8 ? C7 C6 C7 C6 -92.8(17) 2 . . 4 ? N1 C6 C7 C6 -116.8(5) . . . 4 ? C7 C6 C7 C6 -17.8(9) 4 . . 4 ? C6 C6 C7 C6 -94.0(4) 2 . . 4 ? C6 C6 C7 C6 -96(2) 3 . . 4 ? C7 C6 C7 C7 2(2) 2 . . 3 ? N1 C6 C7 C7 -22.2(5) . . . 3 ? C6 C6 C7 C7 94.6(4) 4 . . 3 ? C7 C6 C7 C7 76.8(8) 4 . . 3 ? C6 C6 C7 C7 0.6(7) 2 . . 3 ? C6 C6 C7 C7 -1.5(16) 3 . . 3 ? N1 C6 C7 C7 -24.0(17) . . . 2 ? C6 C6 C7 C7 92.8(17) 4 . . 2 ? C7 C6 C7 C7 75.0(17) 4 . . 2 ? C6 C6 C7 C7 -1.2(13) 2 . . 2 ? C6 C6 C7 C7 -3(4) 3 . . 2 ? C6 C7 N1 C7 -153.1(6) . . . 3 ? C6 C7 N1 C7 12.6(9) 3 . . 3 ? C7 C7 N1 C7 -50.5(9) 8 . . 3 ? C6 C7 N1 C7 -91.4(6) 4 . . 3 ? C7 C7 N1 C7 -139.8(7) 2 . . 3 ? C6 C7 N1 C7 -83.2(7) . . . 6 ? C6 C7 N1 C7 82.5(7) 3 . . 6 ? C7 C7 N1 C7 19.3(7) 8 . . 6 ? C6 C7 N1 C7 -21.5(6) 4 . . 6 ? C7 C7 N1 C7 69.9(4) 3 . . 6 ? C7 C7 N1 C7 -69.9(4) 2 . . 6 ? C6 C7 N1 C7 -13.3(10) . . . 2 ? C6 C7 N1 C7 152.4(6) 3 . . 2 ? C7 C7 N1 C7 89.2(7) 8 . . 2 ? C6 C7 N1 C7 48.4(8) 4 . . 2 ? C7 C7 N1 C7 139.8(7) 3 . . 2 ? C6 C7 N1 C6 165.7(14) 3 . . . ? C7 C7 N1 C6 102.5(12) 8 . . . ? C6 C7 N1 C6 61.7(9) 4 . . . ? C7 C7 N1 C6 153.1(6) 3 . . . ? C7 C7 N1 C6 13.3(10) 2 . . . ? C6 C7 N1 C6 -165.7(14) . . . 3 ? C7 C7 N1 C6 -63.2(9) 8 . . 3 ? C6 C7 N1 C6 -104.0(9) 4 . . 3 ? C7 C7 N1 C6 -12.6(9) 3 . . 3 ? C7 C7 N1 C6 -152.4(6) 2 . . 3 ? C6 C7 N1 C6 -131.6(10) . . . 6 ? C6 C7 N1 C6 34.2(7) 3 . . 6 ? C7 C7 N1 C6 -29.0(10) 8 . . 6 ? C6 C7 N1 C6 -69.9(7) 4 . . 6 ? C7 C7 N1 C6 21.5(4) 3 . . 6 ? C7 C7 N1 C6 -118.2(8) 2 . . 6 ? C6 C7 N1 C6 -32.9(7) . . . 2 ? C6 C7 N1 C6 132.9(10) 3 . . 2 ? C7 C7 N1 C6 69.7(10) 8 . . 2 ? C6 C7 N1 C6 28.8(9) 4 . . 2 ? C7 C7 N1 C6 120.2(8) 3 . . 2 ? C7 C7 N1 C6 -19.5(5) 2 . . 2 ? C6 C7 N1 Zn1 96.8(7) . . . . ? C6 C7 N1 Zn1 -97.5(7) 3 . . . ? C7 C7 N1 Zn1 -160.7(7) 8 . . . ? C6 C7 N1 Zn1 158.5(6) 4 . . . ? C7 C7 N1 Zn1 -110.1(4) 3 . . . ? C7 C7 N1 Zn1 110.1(4) 2 . . . ? C7 C6 N1 C7 -160.5(14) 2 . . . ? C6 C6 N1 C7 -63.1(9) 4 . . . ? C7 C6 N1 C7 -101.0(10) 4 . . . ? C6 C6 N1 C7 -151.2(7) 2 . . . ? C6 C6 N1 C7 -9.8(9) 3 . . . ? C7 C6 N1 C7 30.6(7) . . . 3 ? C7 C6 N1 C7 -129.9(10) 2 . . 3 ? C6 C6 N1 C7 -32.5(9) 4 . . 3 ? C7 C6 N1 C7 -70.3(7) 4 . . 3 ? C6 C6 N1 C7 -120.6(8) 2 . . 3 ? C6 C6 N1 C7 20.8(4) 3 . . 3 ? C7 C6 N1 C7 128.4(11) . . . 6 ? C7 C6 N1 C7 -32.1(6) 2 . . 6 ? C6 C6 N1 C7 65.3(9) 4 . . 6 ? C7 C6 N1 C7 27.5(8) 4 . . 6 ? C6 C6 N1 C7 -22.8(5) 2 . . 6 ? C6 C6 N1 C7 118.6(8) 3 . . 6 ? C7 C6 N1 C7 160.5(14) . . . 2 ? C6 C6 N1 C7 97.4(11) 4 . . 2 ? C7 C6 N1 C7 59.5(9) 4 . . 2 ? C6 C6 N1 C7 9.3(9) 2 . . 2 ? C6 C6 N1 C7 150.7(6) 3 . . 2 ? C7 C6 N1 C6 9.8(9) . . . 3 ? C7 C6 N1 C6 -150.7(6) 2 . . 3 ? C6 C6 N1 C6 -53.3(8) 4 . . 3 ? C7 C6 N1 C6 -91.2(6) 4 . . 3 ? C6 C6 N1 C6 -141.4(7) 2 . . 3 ? C7 C6 N1 C6 80.5(7) . . . 6 ? C7 C6 N1 C6 -80.0(7) 2 . . 6 ? C6 C6 N1 C6 17.4(7) 4 . . 6 ? C7 C6 N1 C6 -20.5(6) 4 . . 6 ? C6 C6 N1 C6 -70.7(3) 2 . . 6 ? C6 C6 N1 C6 70.7(3) 3 . . 6 ? C7 C6 N1 C6 151.2(7) . . . 2 ? C7 C6 N1 C6 -9.3(9) 2 . . 2 ? C6 C6 N1 C6 88.1(6) 4 . . 2 ? C7 C6 N1 C6 50.2(7) 4 . . 2 ? C6 C6 N1 C6 141.4(7) 3 . . 2 ? C7 C6 N1 Zn1 -99.5(7) . . . . ? C7 C6 N1 Zn1 100.0(7) 2 . . . ? C6 C6 N1 Zn1 -162.6(7) 4 . . . ? C7 C6 N1 Zn1 159.5(6) 4 . . . ? C6 C6 N1 Zn1 109.3(3) 2 . . . ? C6 C6 N1 Zn1 -109.3(3) 3 . . . ? O1 Zn1 N1 C7 93.3(5) 6 . . . ? O1 Zn1 N1 C7 3.3(5) 3 . . . ? O1 Zn1 N1 C7 -86.7(5) . . . . ? O1 Zn1 N1 C7 -176.7(5) 2 . . . ? Zn1 Zn1 N1 C7 -124(8) 17 . . . ? O1 Zn1 N1 C7 3.3(5) 6 . . 3 ? O1 Zn1 N1 C7 -86.7(5) 3 . . 3 ? O1 Zn1 N1 C7 -176.7(5) . . . 3 ? O1 Zn1 N1 C7 93.3(5) 2 . . 3 ? Zn1 Zn1 N1 C7 146(8) 17 . . 3 ? O1 Zn1 N1 C7 -86.7(5) 6 . . 6 ? O1 Zn1 N1 C7 -176.7(5) 3 . . 6 ? O1 Zn1 N1 C7 93.3(5) . . . 6 ? O1 Zn1 N1 C7 3.3(5) 2 . . 6 ? Zn1 Zn1 N1 C7 56(8) 17 . . 6 ? O1 Zn1 N1 C7 -176.7(5) 6 . . 2 ? O1 Zn1 N1 C7 93.3(5) 3 . . 2 ? O1 Zn1 N1 C7 3.3(5) . . . 2 ? O1 Zn1 N1 C7 -86.7(5) 2 . . 2 ? Zn1 Zn1 N1 C7 -34(8) 17 . . 2 ? O1 Zn1 N1 C6 136.9(4) 6 . . . ? O1 Zn1 N1 C6 46.9(4) 3 . . . ? O1 Zn1 N1 C6 -43.1(4) . . . . ? O1 Zn1 N1 C6 -133.1(4) 2 . . . ? Zn1 Zn1 N1 C6 -80(8) 17 . . . ? O1 Zn1 N1 C6 46.9(4) 6 . . 3 ? O1 Zn1 N1 C6 -43.1(4) 3 . . 3 ? O1 Zn1 N1 C6 -133.1(4) . . . 3 ? O1 Zn1 N1 C6 136.9(4) 2 . . 3 ? Zn1 Zn1 N1 C6 -170(8) 17 . . 3 ? O1 Zn1 N1 C6 -43.1(4) 6 . . 6 ? O1 Zn1 N1 C6 -133.1(4) 3 . . 6 ? O1 Zn1 N1 C6 136.9(4) . . . 6 ? O1 Zn1 N1 C6 46.9(4) 2 . . 6 ? Zn1 Zn1 N1 C6 100(8) 17 . . 6 ? O1 Zn1 N1 C6 -133.1(4) 6 . . 2 ? O1 Zn1 N1 C6 136.9(4) 3 . . 2 ? O1 Zn1 N1 C6 46.9(4) . . . 2 ? O1 Zn1 N1 C6 -43.1(4) 2 . . 2 ? Zn1 Zn1 N1 C6 10(8) 17 . . 2 ? O1 C1 O1 Zn1 4.0(10) 22 . . . ? C2 C1 O1 Zn1 -178.2(5) . . . . ? O1 Zn1 O1 C1 -1.9(4) 6 . . . ? O1 Zn1 O1 C1 78.3(5) 3 . . . ? O1 Zn1 O1 C1 -82.0(4) 2 . . . ? N1 Zn1 O1 C1 178.1(4) . . . . ? Zn1 Zn1 O1 C1 -1.9(4) 17 . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.86 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.786 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 942883'