# 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H48 N30 O18 Zn3' _chemical_formula_weight 1673.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 cubic _symmetry_space_group_name_H-M Fd-3c 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 0.237 0.006 0.006 5403 446 ' ' 2 0.737 0.006 0.006 5403 446 ' ' _platon_squeeze_details ; ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/4, z+3/4' '-x+1/4, -y+1/4, z' 'y+1/4, -x, z+3/4' 'x+1/4, -z, y+3/4' 'x, -y+1/4, -z+1/4' 'x+1/4, z+3/4, -y' 'z+1/4, y+3/4, -x' '-x+1/4, y, -z+1/4' '-z, y+1/4, x+3/4' 'z, x, y' 'y, z, x' '-y+1/4, -z+1/4, x' 'z, -x+1/4, -y+1/4' '-y+1/4, z, -x+1/4' '-z+1/4, -x+1/4, y' '-z+1/4, x, -y+1/4' 'y, -z+1/4, -x+1/4' 'y+1/4, x+3/4, -z' '-y, -x, -z+1/2' '-x, z+1/4, y+3/4' '-x, -z, -y+1/2' 'z+1/4, -y, x+3/4' '-z, -y, -x+1/2' 'x, y+1/2, z+1/2' '-y, x+3/4, z+5/4' '-x+1/4, -y+3/4, z+1/2' 'y+1/4, -x+1/2, z+5/4' 'x+1/4, -z+1/2, y+5/4' 'x, -y+3/4, -z+3/4' 'x+1/4, z+5/4, -y+1/2' 'z+1/4, y+5/4, -x+1/2' '-x+1/4, y+1/2, -z+3/4' '-z, y+3/4, x+5/4' 'z, x+1/2, y+1/2' 'y, z+1/2, x+1/2' '-y+1/4, -z+3/4, x+1/2' 'z, -x+3/4, -y+3/4' '-y+1/4, z+1/2, -x+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+1/4, x+1/2, -y+3/4' 'y, -z+3/4, -x+3/4' 'y+1/4, x+5/4, -z+1/2' '-y, -x+1/2, -z+1' '-x, z+3/4, y+5/4' '-x, -z+1/2, -y+1' 'z+1/4, -y+1/2, x+5/4' '-z, -y+1/2, -x+1' 'x+1/2, y, z+1/2' '-y+1/2, x+1/4, z+5/4' '-x+3/4, -y+1/4, z+1/2' 'y+3/4, -x, z+5/4' 'x+3/4, -z, y+5/4' 'x+1/2, -y+1/4, -z+3/4' 'x+3/4, z+3/4, -y+1/2' 'z+3/4, y+3/4, -x+1/2' '-x+3/4, y, -z+3/4' '-z+1/2, y+1/4, x+5/4' 'z+1/2, x, y+1/2' 'y+1/2, z, x+1/2' '-y+3/4, -z+1/4, x+1/2' 'z+1/2, -x+1/4, -y+3/4' '-y+3/4, z, -x+3/4' '-z+3/4, -x+1/4, y+1/2' '-z+3/4, x, -y+3/4' 'y+1/2, -z+1/4, -x+3/4' 'y+3/4, x+3/4, -z+1/2' '-y+1/2, -x, -z+1' '-x+1/2, z+1/4, y+5/4' '-x+1/2, -z, -y+1' 'z+3/4, -y, x+5/4' '-z+1/2, -y, -x+1' 'x+1/2, y+1/2, z' '-y+1/2, x+3/4, z+3/4' '-x+3/4, -y+3/4, z' 'y+3/4, -x+1/2, z+3/4' 'x+3/4, -z+1/2, y+3/4' 'x+1/2, -y+3/4, -z+1/4' 'x+3/4, z+5/4, -y' 'z+3/4, y+5/4, -x' '-x+3/4, y+1/2, -z+1/4' '-z+1/2, y+3/4, x+3/4' 'z+1/2, x+1/2, y' 'y+1/2, z+1/2, x' '-y+3/4, -z+3/4, x' 'z+1/2, -x+3/4, -y+1/4' '-y+3/4, z+1/2, -x+1/4' '-z+3/4, -x+3/4, y' '-z+3/4, x+1/2, -y+1/4' 'y+1/2, -z+3/4, -x+1/4' 'y+3/4, x+5/4, -z' '-y+1/2, -x+1/2, -z+1/2' '-x+1/2, z+3/4, y+3/4' '-x+1/2, -z+1/2, -y+1/2' 'z+3/4, -y+1/2, x+3/4' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'y, -x-1/4, -z-3/4' 'x-1/4, y-1/4, -z' '-y-1/4, x, -z-3/4' '-x-1/4, z, -y-3/4' '-x, y-1/4, z-1/4' '-x-1/4, -z-3/4, y' '-z-1/4, -y-3/4, x' 'x-1/4, -y, z-1/4' 'z, -y-1/4, -x-3/4' '-z, -x, -y' '-y, -z, -x' 'y-1/4, z-1/4, -x' '-z, x-1/4, y-1/4' 'y-1/4, -z, x-1/4' 'z-1/4, x-1/4, -y' 'z-1/4, -x, y-1/4' '-y, z-1/4, x-1/4' '-y-1/4, -x-3/4, z' 'y, x, z-1/2' 'x, -z-1/4, -y-3/4' 'x, z, y-1/2' '-z-1/4, y, -x-3/4' 'z, y, x-1/2' '-x, -y+1/2, -z+1/2' 'y, -x+1/4, -z-1/4' 'x-1/4, y+1/4, -z+1/2' '-y-1/4, x+1/2, -z-1/4' '-x-1/4, z+1/2, -y-1/4' '-x, y+1/4, z+1/4' '-x-1/4, -z-1/4, y+1/2' '-z-1/4, -y-1/4, x+1/2' 'x-1/4, -y+1/2, z+1/4' 'z, -y+1/4, -x-1/4' '-z, -x+1/2, -y+1/2' '-y, -z+1/2, -x+1/2' 'y-1/4, z+1/4, -x+1/2' '-z, x+1/4, y+1/4' 'y-1/4, -z+1/2, x+1/4' 'z-1/4, x+1/4, -y+1/2' 'z-1/4, -x+1/2, y+1/4' '-y, z+1/4, x+1/4' '-y-1/4, -x-1/4, z+1/2' 'y, x+1/2, z' 'x, -z+1/4, -y-1/4' 'x, z+1/2, y' '-z-1/4, y+1/2, -x-1/4' 'z, y+1/2, x' '-x+1/2, -y, -z+1/2' 'y+1/2, -x-1/4, -z-1/4' 'x+1/4, y-1/4, -z+1/2' '-y+1/4, x, -z-1/4' '-x+1/4, z, -y-1/4' '-x+1/2, y-1/4, z+1/4' '-x+1/4, -z-3/4, y+1/2' '-z+1/4, -y-3/4, x+1/2' 'x+1/4, -y, z+1/4' 'z+1/2, -y-1/4, -x-1/4' '-z+1/2, -x, -y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/4, z-1/4, -x+1/2' '-z+1/2, x-1/4, y+1/4' 'y+1/4, -z, x+1/4' 'z+1/4, x-1/4, -y+1/2' 'z+1/4, -x, y+1/4' '-y+1/2, z-1/4, x+1/4' '-y+1/4, -x-3/4, z+1/2' 'y+1/2, x, z' 'x+1/2, -z-1/4, -y-1/4' 'x+1/2, z, y' '-z+1/4, y, -x-1/4' 'z+1/2, y, x' '-x+1/2, -y+1/2, -z' 'y+1/2, -x+1/4, -z-3/4' 'x+1/4, y+1/4, -z' '-y+1/4, x+1/2, -z-3/4' '-x+1/4, z+1/2, -y-3/4' '-x+1/2, y+1/4, z-1/4' '-x+1/4, -z-1/4, y' '-z+1/4, -y-1/4, x' 'x+1/4, -y+1/2, z-1/4' 'z+1/2, -y+1/4, -x-3/4' '-z+1/2, -x+1/2, -y' '-y+1/2, -z+1/2, -x' 'y+1/4, z+1/4, -x' '-z+1/2, x+1/4, y-1/4' 'y+1/4, -z+1/2, x-1/4' 'z+1/4, x+1/4, -y' 'z+1/4, -x+1/2, y-1/4' '-y+1/2, z+1/4, x-1/4' '-y+1/4, -x-1/4, z' 'y+1/2, x+1/2, z-1/2' 'x+1/2, -z+1/4, -y-3/4' 'x+1/2, z+1/2, y-1/2' '-z+1/4, y+1/2, -x-3/4' 'z+1/2, y+1/2, x-1/2' _cell_length_a 32.702(3) _cell_length_b 32.702(3) _cell_length_c 32.702(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 34973(5) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24741 _cell_measurement_theta_min 2.0647 _cell_measurement_theta_max 27.4778 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13632 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5421 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn724HG _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54485 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1293 _reflns_number_gt 1281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1103P)^2^+584.1537P] 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 1293 _refine_ls_number_parameters 98 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2426 _refine_ls_wR_factor_gt 0.2419 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.192 _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 Zn1 Zn 0.6250 0.3750 0.1250 0.0426(6) Uani 1 4 d S . . C1 C 0.7041(3) 0.3295(3) 0.1316(3) 0.106(3) Uani 1 1 d U . . H1A H 0.7118 0.3431 0.1561 0.127 Uiso 1 1 calc R . . C2 C 0.7260(3) 0.2997(3) 0.1133(3) 0.105(3) Uani 1 1 d U . . H2A H 0.7525 0.2903 0.1209 0.126 Uiso 1 1 calc R . . C3 C 0.6695(2) 0.31001(19) 0.08113(19) 0.0584(17) Uani 1 1 d . . . H3A H 0.6481 0.3075 0.0616 0.070 Uiso 1 1 calc R . . C4 C 0.7113(2) 0.25220(19) 0.0558(2) 0.0556(17) Uani 1 1 d . . . C5 C 0.6861(2) 0.24437(19) 0.0225(2) 0.0598(19) Uani 1 1 d . . . H5A H 0.6634 0.2617 0.0169 0.072 Uiso 1 1 calc R . . N1 N 0.66981(17) 0.33707(16) 0.11030(18) 0.0576(15) Uani 1 1 d . . . N2 N 0.70284(16) 0.28604(16) 0.08190(18) 0.0615(16) Uani 1 1 d . . . N3 N 0.7500 0.4194(3) 0.0806(3) 0.090(3) Uani 1 2 d SD . . O1 O 0.7322(7) 0.4439(6) 0.0996(6) 0.129(7) Uani 0.50 1 d PD . . O2 O 0.7408(6) 0.3899(5) 0.0608(6) 0.114(6) Uani 0.50 1 d PD . . O3 O 0.7906(4) 0.4228(7) 0.0835(9) 0.175(9) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0509(7) 0.0259(7) 0.0509(7) 0.000 0.000 0.000 C1 0.105(5) 0.102(5) 0.111(5) -0.051(4) -0.037(4) 0.025(4) C2 0.092(5) 0.106(5) 0.117(5) -0.052(4) -0.038(4) 0.030(4) C3 0.066(4) 0.058(4) 0.051(4) -0.019(3) -0.020(3) 0.017(3) C4 0.058(4) 0.049(3) 0.060(4) -0.020(3) -0.017(3) 0.018(3) C5 0.061(4) 0.054(4) 0.064(4) -0.029(3) -0.026(3) 0.024(3) N1 0.057(3) 0.050(3) 0.066(3) -0.023(3) -0.021(3) 0.023(3) N2 0.057(3) 0.054(3) 0.074(4) -0.030(3) -0.027(3) 0.023(3) N3 0.088(8) 0.091(5) 0.091(5) -0.021(6) 0.006(5) 0.006(5) O1 0.117(14) 0.143(15) 0.127(15) -0.064(12) 0.033(13) 0.035(14) O2 0.105(13) 0.123(13) 0.114(13) -0.062(11) -0.015(11) 0.012(12) O3 0.104(14) 0.170(19) 0.25(3) -0.049(19) -0.012(17) 0.013(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.979(5) 128_664 ? Zn1 N1 1.979(5) . ? Zn1 N1 1.979(5) 9_655 ? Zn1 N1 1.979(5) 154_566 ? C1 N1 1.343(11) . ? C1 C2 1.350(13) . ? C1 H1A 0.9500 . ? C2 N2 1.353(10) . ? C2 H2A 0.9500 . ? C3 N1 1.301(8) . ? C3 N2 1.344(8) . ? C3 H3A 0.9500 . ? C4 C5 1.377(8) 66 ? C4 C5 1.390(8) . ? C4 N2 1.424(7) . ? C5 C4 1.377(8) 89_545 ? C5 H5A 0.9500 . ? N3 O1 1.167(12) . ? N3 O1 1.167(12) 94_655 ? N3 O2 1.201(13) 94_655 ? N3 O2 1.201(13) . ? N3 O3 1.335(13) . ? N3 O3 1.335(12) 94_655 ? O1 O2 0.96(2) 94_655 ? O1 O3 1.38(2) 94_655 ? O2 O1 0.96(2) 94_655 ? O2 O3 1.45(2) 94_655 ? O3 O1 1.38(2) 94_655 ? O3 O2 1.45(2) 94_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 113.13(19) 128_664 . ? N1 Zn1 N1 113.13(19) 128_664 9_655 ? N1 Zn1 N1 102.4(4) . 9_655 ? N1 Zn1 N1 102.4(4) 128_664 154_566 ? N1 Zn1 N1 113.13(19) . 154_566 ? N1 Zn1 N1 113.13(19) 9_655 154_566 ? N1 C1 C2 110.3(8) . . ? N1 C1 H1A 124.9 . . ? C2 C1 H1A 124.9 . . ? C1 C2 N2 106.1(8) . . ? C1 C2 H2A 127.0 . . ? N2 C2 H2A 127.0 . . ? N1 C3 N2 112.1(6) . . ? N1 C3 H3A 124.0 . . ? N2 C3 H3A 124.0 . . ? C5 C4 C5 120.6(6) 66 . ? C5 C4 N2 119.6(5) 66 . ? C5 C4 N2 119.8(5) . . ? C4 C5 C4 119.4(6) 89_545 . ? C4 C5 H5A 120.3 89_545 . ? C4 C5 H5A 120.3 . . ? C3 N1 C1 105.2(6) . . ? C3 N1 Zn1 126.7(4) . . ? C1 N1 Zn1 127.4(5) . . ? C3 N2 C2 106.1(6) . . ? C3 N2 C4 126.8(5) . . ? C2 N2 C4 127.1(6) . . ? O1 N3 O1 167(3) . 94_655 ? O1 N3 O2 47.7(9) . 94_655 ? O1 N3 O2 135.5(10) 94_655 94_655 ? O1 N3 O2 135.5(10) . . ? O1 N3 O2 47.7(9) 94_655 . ? O2 N3 O2 159(2) 94_655 . ? O1 N3 O3 113.5(11) . . ? O1 N3 O3 66.3(11) 94_655 . ? O2 N3 O3 69.5(11) 94_655 . ? O2 N3 O3 110.7(10) . . ? O1 N3 O3 66.3(11) . 94_655 ? O1 N3 O3 113.5(11) 94_655 94_655 ? O2 N3 O3 110.7(10) 94_655 94_655 ? O2 N3 O3 69.5(11) . 94_655 ? O3 N3 O3 179(3) . 94_655 ? O2 O1 N3 68.0(12) 94_655 . ? O2 O1 O3 126(2) 94_655 94_655 ? N3 O1 O3 62.7(10) . 94_655 ? O1 O2 N3 64.3(12) 94_655 . ? O1 O2 O3 120(2) 94_655 94_655 ? N3 O2 O3 59.6(10) . 94_655 ? N3 O3 O1 51.0(7) . 94_655 ? N3 O3 O2 50.9(7) . 94_655 ? O1 O3 O2 101.8(12) 94_655 94_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.572 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 944998' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 Cl4 N18 O16 Zn2' _chemical_formula_weight 1357.46 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.004 -0.011 0.002 4493.2 1523.0 _platon_squeeze_details ; ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.703(3) _cell_length_b 20.062(3) _cell_length_c 22.121(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.799(2) _cell_angle_gamma 90.00 _cell_volume 9118(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25076 _cell_measurement_theta_min 2.0303 _cell_measurement_theta_max 27.4854 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn724HG _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63611 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16047 _reflns_number_gt 13554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^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 16047 _refine_ls_number_parameters 812 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1425 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.139367(14) 0.662554(14) 0.944142(14) 0.01847(10) Uani 1 1 d . . . Zn2 Zn 0.602024(16) 0.862189(14) 0.740175(15) 0.02213(11) Uani 1 1 d . . . C1 C 0.27805(13) 0.42294(13) 1.02273(13) 0.0227(6) Uani 1 1 d . . . C2 C 0.29995(13) 0.40663(13) 0.97331(13) 0.0242(6) Uani 1 1 d . . . H2A H 0.3007 0.4387 0.9420 0.029 Uiso 1 1 calc R . . C3 C 0.32133(13) 0.34090(13) 0.97001(13) 0.0220(6) Uani 1 1 d . . . C4 C 0.32219(14) 0.29411(13) 1.01674(13) 0.0246(6) Uani 1 1 d . . . H4A H 0.3382 0.2503 1.0152 0.030 Uiso 1 1 calc R . . C5 C 0.29903(14) 0.31318(14) 1.06545(13) 0.0246(6) Uani 1 1 d . . . C6 C 0.27652(14) 0.37732(14) 1.06981(13) 0.0257(6) Uani 1 1 d . . . H6A H 0.2607 0.3896 1.1036 0.031 Uiso 1 1 calc R . . C7 C 0.21487(14) 0.52510(13) 0.97968(13) 0.0250(6) Uani 1 1 d . . . H7A H 0.1987 0.5108 0.9365 0.030 Uiso 1 1 calc R . . C8 C 0.23513(14) 0.58377(14) 1.06562(14) 0.0284(6) Uani 1 1 d . . . H8A H 0.2353 0.6196 1.0938 0.034 Uiso 1 1 calc R . . C9 C 0.26861(15) 0.52636(14) 1.08293(14) 0.0294(6) Uani 1 1 d . . . H9A H 0.2955 0.5142 1.1246 0.035 Uiso 1 1 calc R . . C10 C 0.36852(14) 0.36260(13) 0.88340(13) 0.0233(6) Uani 1 1 d . . . H10A H 0.3753 0.4091 0.8907 0.028 Uiso 1 1 calc R . . C11 C 0.36491(16) 0.26281(13) 0.84424(14) 0.0304(7) Uani 1 1 d . . . H11A H 0.3689 0.2269 0.8178 0.036 Uiso 1 1 calc R . . C12 C 0.34263(16) 0.25792(14) 0.89432(14) 0.0317(7) Uani 1 1 d . . . H12A H 0.3284 0.2185 0.9097 0.038 Uiso 1 1 calc R . . C13 C 0.34999(14) 0.22636(13) 1.14500(13) 0.0246(6) Uani 1 1 d . . . H13A H 0.3893 0.2227 1.1351 0.029 Uiso 1 1 calc R . . C14 C 0.27518(15) 0.21256(15) 1.18958(15) 0.0328(7) Uani 1 1 d . . . H14A H 0.2532 0.1965 1.2175 0.039 Uiso 1 1 calc R . . C15 C 0.25106(15) 0.25817(16) 1.14274(15) 0.0334(7) Uani 1 1 d . . . H15A H 0.2100 0.2798 1.1316 0.040 Uiso 1 1 calc R . . C16 C 0.04556(13) 0.64368(13) 1.14492(13) 0.0217(5) Uani 1 1 d . . . C17 C 0.01555(13) 0.58154(13) 1.13485(12) 0.0220(5) Uani 1 1 d . . . H17A H 0.0102 0.5577 1.0964 0.026 Uiso 1 1 calc R . . C18 C -0.00648(13) 0.55491(13) 1.18216(12) 0.0225(5) Uani 1 1 d . . . C19 C 0.00012(13) 0.58971(13) 1.23823(13) 0.0237(6) Uani 1 1 d . . . H19A H -0.0162 0.5718 1.2698 0.028 Uiso 1 1 calc R . . C20 C 0.03069(14) 0.65049(14) 1.24695(13) 0.0246(6) Uani 1 1 d . . . C21 C 0.05350(13) 0.67941(14) 1.20056(13) 0.0241(6) Uani 1 1 d . . . H21A H 0.0737 0.7220 1.2070 0.029 Uiso 1 1 calc R . . C22 C 0.09105(13) 0.64176(13) 1.05534(12) 0.0208(5) Uani 1 1 d . . . H22A H 0.0966 0.5949 1.0540 0.025 Uiso 1 1 calc R . . C23 C 0.08913(15) 0.74761(13) 1.03464(14) 0.0287(6) Uani 1 1 d . . . H23A H 0.0939 0.7888 1.0154 0.034 Uiso 1 1 calc R . . C24 C 0.06430(16) 0.74056(14) 1.08272(14) 0.0310(7) Uani 1 1 d . . . H24A H 0.0486 0.7751 1.1033 0.037 Uiso 1 1 calc R . . C25 C -0.06775(13) 0.46092(13) 1.11602(13) 0.0242(6) Uani 1 1 d . . . H25A H -0.0701 0.4788 1.0756 0.029 Uiso 1 1 calc R . . C26 C -0.07911(14) 0.39675(14) 1.19021(13) 0.0259(6) Uani 1 1 d . . . H26A H -0.0917 0.3600 1.2107 0.031 Uiso 1 1 calc R . . C27 C -0.04519(15) 0.44996(14) 1.22019(14) 0.0302(6) Uani 1 1 d . . . H27A H -0.0295 0.4577 1.2649 0.036 Uiso 1 1 calc R . . C28 C 0.08948(13) 0.72379(13) 1.33797(13) 0.0246(6) Uani 1 1 d . . . H28A H 0.1294 0.7259 1.3289 0.029 Uiso 1 1 calc R . . C29 C 0.01552(16) 0.73948(17) 1.38178(15) 0.0365(7) Uani 1 1 d . . . H29A H -0.0063 0.7548 1.4101 0.044 Uiso 1 1 calc R . . C30 C -0.01049(16) 0.69781(19) 1.33165(16) 0.0418(8) Uani 1 1 d . . . H30A H -0.0531 0.6794 1.3182 0.050 Uiso 1 1 calc R . . C31 C 0.32786(13) 0.70216(13) 0.83517(13) 0.0226(5) Uani 1 1 d . . . C32 C 0.36030(13) 0.75571(12) 0.81905(13) 0.0226(5) Uani 1 1 d . . . H32A H 0.3591 0.7989 0.8362 0.027 Uiso 1 1 calc R . . C33 C 0.39468(13) 0.74337(13) 0.77654(13) 0.0234(6) Uani 1 1 d . . . C34 C 0.39561(13) 0.68086(13) 0.74971(13) 0.0244(6) Uani 1 1 d . . . H34A H 0.4182 0.6736 0.7199 0.029 Uiso 1 1 calc R . . C35 C 0.36241(13) 0.62918(12) 0.76787(13) 0.0214(5) Uani 1 1 d . . . C36 C 0.32849(13) 0.63855(12) 0.81035(13) 0.0219(5) Uani 1 1 d . . . H36A H 0.3063 0.6027 0.8223 0.026 Uiso 1 1 calc R . . C37 C 0.23997(12) 0.67827(13) 0.88072(13) 0.0214(5) Uani 1 1 d . . . H37A H 0.2208 0.6426 0.8528 0.026 Uiso 1 1 calc R . . C38 C 0.26062(14) 0.75252(14) 0.95557(14) 0.0286(6) Uani 1 1 d . . . H38A H 0.2574 0.7782 0.9905 0.034 Uiso 1 1 calc R . . C39 C 0.30630(14) 0.76037(14) 0.92763(14) 0.0292(6) Uani 1 1 d . . . H39A H 0.3406 0.7921 0.9385 0.035 Uiso 1 1 calc R . . C40 C 0.49042(14) 0.78810(14) 0.75507(14) 0.0265(6) Uani 1 1 d . . . H40A H 0.5135 0.7471 0.7605 0.032 Uiso 1 1 calc R . . C41 C 0.46376(16) 0.89282(14) 0.73821(16) 0.0343(7) Uani 1 1 d . . . H41A H 0.4660 0.9390 0.7296 0.041 Uiso 1 1 calc R . . C42 C 0.41312(16) 0.86215(14) 0.74898(17) 0.0336(7) Uani 1 1 d . . . H42A H 0.3735 0.8822 0.7491 0.040 Uiso 1 1 calc R . . C43 C 0.37442(13) 0.50765(12) 0.77518(13) 0.0217(5) Uani 1 1 d . . . H43A H 0.3766 0.5041 0.8187 0.026 Uiso 1 1 calc R . . C44 C 0.37537(19) 0.48346(15) 0.67992(15) 0.0377(8) Uani 1 1 d . . . H44A H 0.3786 0.4592 0.6442 0.045 Uiso 1 1 calc R . . C45 C 0.36500(18) 0.55009(15) 0.68138(15) 0.0370(7) Uani 1 1 d . . . H45A H 0.3590 0.5807 0.6472 0.044 Uiso 1 1 calc R . . N1 N 0.20057(11) 0.58302(11) 1.00101(11) 0.0227(5) Uani 1 1 d . . . N2 N 0.25578(11) 0.48904(11) 1.02799(11) 0.0231(5) Uani 1 1 d . . . N3 N 0.38121(12) 0.32940(11) 0.83737(11) 0.0237(5) Uani 1 1 d . . . N4 N 0.34449(12) 0.32168(11) 0.91888(11) 0.0234(5) Uani 1 1 d . . . N5 N 0.33673(12) 0.19280(11) 1.19065(11) 0.0243(5) Uani 1 1 d . . . N6 N 0.29961(12) 0.26677(11) 1.11415(11) 0.0258(5) Uani 1 1 d . . . N7 N 0.10675(11) 0.68539(11) 1.01742(10) 0.0212(5) Uani 1 1 d . . . N8 N 0.06603(11) 0.67372(11) 1.09628(10) 0.0211(5) Uani 1 1 d . . . N9 N -0.09299(11) 0.40386(11) 1.12464(11) 0.0230(5) Uani 1 1 d . . . N10 N -0.03766(11) 0.49108(11) 1.17315(10) 0.0214(5) Uani 1 1 d . . . N11 N 0.07761(11) 0.75613(11) 1.38561(11) 0.0233(5) Uani 1 1 d . . . N12 N 0.03734(12) 0.68774(12) 1.30426(11) 0.0266(5) Uani 1 1 d . . . N13 N 0.21858(11) 0.70127(10) 0.92616(10) 0.0203(5) Uani 1 1 d . . . N14 N 0.29360(10) 0.71301(10) 0.87951(11) 0.0208(5) Uani 1 1 d . . . N15 N 0.51243(12) 0.84610(11) 0.74173(12) 0.0270(5) Uani 1 1 d . . . N16 N 0.43012(12) 0.79605(11) 0.75974(12) 0.0264(5) Uani 1 1 d . . . N17 N 0.38042(12) 0.45686(11) 0.73863(11) 0.0260(5) Uani 1 1 d . . . N18 N 0.36483(11) 0.56430(10) 0.74172(11) 0.0215(5) Uani 1 1 d . . . O1 O 0.56279(16) 0.64713(13) 0.82859(15) 0.0610(8) Uani 1 1 d . . . O2 O 0.6001(2) 0.64189(17) 0.7427(2) 0.0913(13) Uani 1 1 d . . . O3 O 0.51249(13) 0.57555(14) 0.74275(15) 0.0622(8) Uani 1 1 d . . . O4 O 0.61522(17) 0.54974(14) 0.81044(16) 0.0795(11) Uani 1 1 d . . . O5 O 0.1712(3) 0.4366(3) 0.8423(3) 0.088(2) Uani 0.646(8) 1 d P A 1 O6 O 0.2229(5) 0.5157(5) 0.8064(6) 0.115(4) Uani 0.646(8) 1 d PU A 1 O7 O 0.1399(6) 0.4516(7) 0.7344(4) 0.078(3) Uani 0.646(8) 1 d P A 1 O8 O 0.2428(5) 0.4057(5) 0.7866(5) 0.054(2) Uani 0.646(8) 1 d P A 1 Cl2 Cl 0.1949(2) 0.4519(3) 0.7898(3) 0.0443(9) Uani 0.646(8) 1 d P A 1 O5A O 0.2243(4) 0.5007(5) 0.7357(4) 0.074(4) Uani 0.354(8) 1 d P A 2 O6A O 0.2188(8) 0.5025(7) 0.8327(5) 0.075(4) Uani 0.354(8) 1 d PU A 2 O7A O 0.1410(6) 0.4409(8) 0.7536(7) 0.045(3) Uani 0.354(8) 1 d PU A 2 O8A O 0.2535(12) 0.4014(14) 0.8016(13) 0.113(9) Uani 0.354(8) 1 d P A 2 Cl2A Cl 0.2084(4) 0.4611(4) 0.7809(4) 0.0322(12) Uani 0.354(8) 1 d P A 2 O9 O 0.5633(2) 0.8295(2) 0.99838(18) 0.0986(12) Uani 1 1 d U . . O10 O 0.5462(2) 0.88138(18) 0.9001(2) 0.1047(13) Uani 1 1 d U . . O11 O 0.52046(14) 0.77091(13) 0.90272(14) 0.0566(7) Uani 1 1 d . . . O12 O 0.45757(15) 0.85316(17) 0.93175(17) 0.0738(10) Uani 1 1 d . . . O13 O 0.14203(15) 0.3816(2) 1.10813(16) 0.0809(10) Uani 1 1 d . . . O14 O 0.0529(3) 0.3559(3) 1.0247(3) 0.167(2) Uani 1 1 d U . . O15 O 0.1097(3) 0.4456(4) 1.0215(3) 0.192(2) Uani 1 1 d U . . O16 O 0.0461(4) 0.4380(6) 1.0722(7) 0.338(8) Uani 1 1 d . . . Cl1 Cl 0.57279(4) 0.60276(3) 0.78161(4) 0.03312(18) Uani 1 1 d . . . Cl3 Cl 0.52183(4) 0.83437(4) 0.93401(4) 0.0401(2) Uani 1 1 d . . . Cl4 Cl 0.09016(4) 0.40651(4) 1.05689(4) 0.0446(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02359(17) 0.01758(17) 0.01728(17) -0.00070(10) 0.01083(13) -0.00124(11) Zn2 0.03228(19) 0.01561(17) 0.02420(19) 0.00251(11) 0.01704(14) -0.00096(12) C1 0.0264(13) 0.0182(12) 0.0249(14) 0.0030(10) 0.0104(11) 0.0037(10) C2 0.0287(14) 0.0243(13) 0.0214(14) 0.0037(10) 0.0103(11) 0.0031(11) C3 0.0289(14) 0.0202(13) 0.0212(14) 0.0034(10) 0.0140(11) 0.0023(10) C4 0.0323(15) 0.0227(13) 0.0208(13) 0.0018(10) 0.0112(11) 0.0036(11) C5 0.0306(14) 0.0255(13) 0.0209(14) 0.0054(11) 0.0125(11) 0.0041(11) C6 0.0299(14) 0.0289(14) 0.0221(14) 0.0039(11) 0.0136(11) 0.0037(11) C7 0.0351(15) 0.0240(13) 0.0182(13) 0.0028(10) 0.0119(11) 0.0024(11) C8 0.0341(15) 0.0262(14) 0.0238(15) -0.0039(11) 0.0080(12) 0.0029(12) C9 0.0369(16) 0.0287(15) 0.0212(14) -0.0012(11) 0.0075(12) 0.0092(12) C10 0.0333(15) 0.0191(13) 0.0220(14) 0.0013(10) 0.0150(12) 0.0007(11) C11 0.0506(18) 0.0183(13) 0.0293(16) -0.0007(11) 0.0228(14) 0.0053(13) C12 0.0524(19) 0.0171(13) 0.0321(16) 0.0003(11) 0.0227(14) 0.0020(12) C13 0.0329(15) 0.0182(13) 0.0280(14) 0.0029(10) 0.0173(12) 0.0061(11) C14 0.0365(16) 0.0359(16) 0.0338(17) 0.0085(13) 0.0220(13) -0.0015(13) C15 0.0338(16) 0.0398(16) 0.0357(17) 0.0128(13) 0.0239(13) 0.0072(13) C16 0.0245(13) 0.0234(13) 0.0186(13) 0.0006(10) 0.0087(11) -0.0009(11) C17 0.0241(13) 0.0248(13) 0.0178(13) -0.0038(10) 0.0076(10) -0.0041(11) C18 0.0264(13) 0.0233(13) 0.0192(13) -0.0033(10) 0.0094(11) -0.0040(11) C19 0.0289(14) 0.0248(14) 0.0202(13) -0.0018(10) 0.0120(11) -0.0060(11) C20 0.0273(14) 0.0306(14) 0.0173(13) -0.0074(11) 0.0092(11) -0.0069(11) C21 0.0273(14) 0.0250(13) 0.0221(14) -0.0035(11) 0.0108(11) -0.0071(11) C22 0.0249(13) 0.0212(13) 0.0196(13) 0.0001(10) 0.0117(11) 0.0008(10) C23 0.0475(18) 0.0188(13) 0.0246(14) -0.0025(10) 0.0182(13) -0.0028(12) C24 0.0492(18) 0.0223(14) 0.0280(15) -0.0038(11) 0.0218(14) -0.0009(13) C25 0.0282(14) 0.0259(14) 0.0181(13) -0.0014(10) 0.0070(11) -0.0017(11) C26 0.0362(15) 0.0246(13) 0.0197(14) 0.0006(10) 0.0130(11) -0.0054(12) C27 0.0428(17) 0.0275(14) 0.0207(14) -0.0010(11) 0.0110(12) -0.0058(13) C28 0.0264(14) 0.0270(14) 0.0255(14) -0.0060(11) 0.0155(11) -0.0086(11) C29 0.0369(16) 0.0503(19) 0.0309(16) -0.0180(14) 0.0227(14) -0.0133(14) C30 0.0358(17) 0.067(2) 0.0306(17) -0.0230(15) 0.0219(14) -0.0234(16) C31 0.0251(13) 0.0198(13) 0.0256(14) -0.0005(10) 0.0119(11) -0.0003(10) C32 0.0259(13) 0.0138(12) 0.0333(15) -0.0031(10) 0.0165(11) -0.0010(10) C33 0.0262(13) 0.0176(12) 0.0305(15) 0.0014(10) 0.0149(11) -0.0001(10) C34 0.0312(15) 0.0198(13) 0.0286(15) 0.0021(11) 0.0187(12) 0.0020(11) C35 0.0229(13) 0.0160(12) 0.0254(14) -0.0009(10) 0.0077(11) 0.0002(10) C36 0.0233(13) 0.0167(12) 0.0276(14) -0.0011(10) 0.0111(11) -0.0026(10) C37 0.0216(13) 0.0222(12) 0.0218(13) -0.0001(10) 0.0092(11) -0.0020(10) C38 0.0295(15) 0.0278(14) 0.0308(15) -0.0124(12) 0.0131(12) -0.0060(12) C39 0.0284(14) 0.0264(14) 0.0336(16) -0.0125(12) 0.0113(12) -0.0102(12) C40 0.0312(15) 0.0211(13) 0.0359(16) 0.0041(11) 0.0229(13) 0.0012(11) C41 0.0423(17) 0.0156(13) 0.053(2) 0.0085(12) 0.0270(15) 0.0034(12) C42 0.0346(16) 0.0200(14) 0.055(2) 0.0046(13) 0.0261(15) 0.0090(12) C43 0.0306(14) 0.0168(12) 0.0202(13) -0.0001(10) 0.0117(11) 0.0007(10) C44 0.074(2) 0.0245(14) 0.0239(15) -0.0012(11) 0.0281(16) 0.0035(15) C45 0.067(2) 0.0258(15) 0.0242(15) 0.0053(12) 0.0230(15) 0.0069(14) N1 0.0257(11) 0.0229(11) 0.0212(11) 0.0004(9) 0.0101(9) 0.0042(9) N2 0.0297(12) 0.0212(11) 0.0205(11) 0.0036(9) 0.0110(9) 0.0059(9) N3 0.0323(12) 0.0195(11) 0.0242(12) -0.0016(9) 0.0161(10) 0.0012(9) N4 0.0324(12) 0.0209(11) 0.0202(11) 0.0026(9) 0.0130(10) 0.0042(9) N5 0.0346(13) 0.0191(11) 0.0234(12) 0.0032(9) 0.0151(10) 0.0011(9) N6 0.0327(13) 0.0264(12) 0.0241(12) 0.0073(9) 0.0174(10) 0.0055(10) N7 0.0276(11) 0.0201(11) 0.0176(11) 0.0020(8) 0.0095(9) 0.0003(9) N8 0.0263(11) 0.0225(11) 0.0175(11) -0.0029(8) 0.0111(9) -0.0027(9) N9 0.0294(12) 0.0219(11) 0.0208(11) 0.0021(9) 0.0123(9) -0.0004(9) N10 0.0255(11) 0.0193(11) 0.0208(11) -0.0028(8) 0.0093(9) -0.0066(9) N11 0.0268(12) 0.0241(11) 0.0193(11) -0.0051(9) 0.0076(9) -0.0047(9) N12 0.0354(13) 0.0276(12) 0.0217(12) -0.0081(9) 0.0158(10) -0.0094(10) N13 0.0245(11) 0.0164(10) 0.0220(11) -0.0029(8) 0.0101(9) -0.0013(8) N14 0.0220(11) 0.0184(10) 0.0263(12) -0.0035(9) 0.0139(9) -0.0036(9) N15 0.0352(13) 0.0161(10) 0.0366(14) 0.0015(9) 0.0210(11) -0.0015(9) N16 0.0293(12) 0.0158(11) 0.0416(14) 0.0040(9) 0.0218(11) 0.0001(9) N17 0.0372(13) 0.0198(11) 0.0253(12) -0.0016(9) 0.0163(10) 0.0015(10) N18 0.0288(12) 0.0131(10) 0.0266(12) -0.0015(8) 0.0144(10) 0.0007(9) O1 0.081(2) 0.0404(14) 0.075(2) -0.0201(13) 0.0439(17) -0.0089(14) O2 0.130(3) 0.071(2) 0.106(3) 0.0200(19) 0.084(3) -0.021(2) O3 0.0406(14) 0.0550(16) 0.080(2) -0.0157(14) 0.0047(14) -0.0024(12) O4 0.077(2) 0.0449(16) 0.085(2) 0.0031(15) -0.0173(18) 0.0297(15) O5 0.078(4) 0.137(6) 0.054(3) -0.024(3) 0.028(3) 0.007(4) O6 0.088(5) 0.082(5) 0.180(9) -0.023(6) 0.048(6) -0.025(4) O7 0.068(5) 0.110(7) 0.048(5) 0.013(4) 0.009(3) 0.021(4) O8 0.028(3) 0.053(4) 0.073(5) -0.023(4) 0.006(3) 0.020(2) Cl2 0.0366(18) 0.0378(15) 0.061(2) -0.0093(11) 0.0186(11) -0.0016(11) O5A 0.045(5) 0.103(7) 0.060(6) 0.050(5) -0.004(4) -0.023(5) O6A 0.110(8) 0.070(7) 0.035(5) -0.033(5) 0.007(5) 0.011(6) O7A 0.013(4) 0.055(5) 0.060(8) 0.008(6) 0.000(5) -0.004(3) O8A 0.073(13) 0.098(12) 0.135(18) 0.045(10) -0.010(10) 0.014(9) Cl2A 0.024(3) 0.034(2) 0.038(2) -0.0039(15) 0.0093(17) -0.0038(17) O9 0.092(2) 0.130(2) 0.0608(18) -0.0124(18) 0.0068(16) 0.044(2) O10 0.154(3) 0.0585(19) 0.134(3) 0.008(2) 0.091(3) -0.017(2) O11 0.0593(16) 0.0471(15) 0.0734(19) -0.0149(13) 0.0354(15) -0.0002(13) O12 0.0521(18) 0.092(2) 0.076(2) -0.0279(18) 0.0189(16) 0.0202(16) O13 0.0520(18) 0.120(3) 0.0584(19) 0.0174(19) 0.0008(15) 0.0280(19) O14 0.164(4) 0.145(4) 0.138(4) 0.010(3) -0.026(3) -0.065(3) O15 0.167(3) 0.208(3) 0.188(3) 0.129(3) 0.041(3) -0.037(3) O16 0.163(7) 0.369(13) 0.474(18) -0.138(13) 0.091(9) 0.151(8) Cl1 0.0349(4) 0.0259(3) 0.0400(4) 0.0041(3) 0.0140(3) 0.0011(3) Cl3 0.0454(5) 0.0448(5) 0.0334(4) -0.0011(3) 0.0172(4) 0.0089(3) Cl4 0.0295(4) 0.0470(5) 0.0508(5) 0.0032(4) 0.0041(3) 0.0004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N7 2.019(2) . ? Zn1 N9 2.029(2) 3_567 ? Zn1 N13 2.039(2) . ? Zn1 N1 2.194(2) . ? Zn1 N11 2.240(2) 4_575 ? Zn2 N17 1.964(2) 2_656 ? Zn2 N3 1.977(2) 2_656 ? Zn2 N15 1.982(3) . ? Zn2 N5 2.004(2) 3_667 ? C1 C2 1.365(4) . ? C1 C6 1.395(4) . ? C1 N2 1.429(3) . ? C2 C3 1.408(4) . ? C2 H2A 0.9500 . ? C3 C4 1.392(4) . ? C3 N4 1.431(4) . ? C4 C5 1.382(4) . ? C4 H4A 0.9500 . ? C5 C6 1.391(4) . ? C5 N6 1.421(3) . ? C6 H6A 0.9500 . ? C7 N1 1.328(4) . ? C7 N2 1.357(4) . ? C7 H7A 0.9500 . ? C8 C9 1.350(4) . ? C8 N1 1.384(4) . ? C8 H8A 0.9500 . ? C9 N2 1.377(4) . ? C9 H9A 0.9500 . ? C10 N3 1.318(3) . ? C10 N4 1.351(4) . ? C10 H10A 0.9500 . ? C11 C12 1.348(4) . ? C11 N3 1.403(4) . ? C11 H11A 0.9500 . ? C12 N4 1.385(4) . ? C12 H12A 0.9500 . ? C13 N5 1.320(3) . ? C13 N6 1.355(4) . ? C13 H13A 0.9500 . ? C14 C15 1.355(4) . ? C14 N5 1.386(4) . ? C14 H14A 0.9500 . ? C15 N6 1.404(4) . ? C15 H15A 0.9500 . ? C16 C21 1.386(4) . ? C16 C17 1.391(4) . ? C16 N8 1.423(3) . ? C17 C18 1.390(4) . ? C17 H17A 0.9500 . ? C18 C19 1.390(4) . ? C18 N10 1.432(3) . ? C19 C20 1.372(4) . ? C19 H19A 0.9500 . ? C20 C21 1.401(4) . ? C20 N12 1.438(3) . ? C21 H21A 0.9500 . ? C22 N7 1.330(3) . ? C22 N8 1.358(3) . ? C22 H22A 0.9500 . ? C23 C24 1.346(4) . ? C23 N7 1.394(3) . ? C23 H23A 0.9500 . ? C24 N8 1.372(4) . ? C24 H24A 0.9500 . ? C25 N9 1.309(4) . ? C25 N10 1.363(3) . ? C25 H25A 0.9500 . ? C26 C27 1.344(4) . ? C26 N9 1.391(4) . ? C26 H26A 0.9500 . ? C27 N10 1.378(4) . ? C27 H27A 0.9500 . ? C28 N11 1.332(4) . ? C28 N12 1.347(4) . ? C28 H28A 0.9500 . ? C29 C30 1.358(4) . ? C29 N11 1.364(4) . ? C29 H29A 0.9500 . ? C30 N12 1.375(4) . ? C30 H30A 0.9500 . ? C31 C36 1.391(4) . ? C31 C32 1.392(4) . ? C31 N14 1.425(4) . ? C32 C33 1.398(4) . ? C32 H32A 0.9500 . ? C33 C34 1.390(4) . ? C33 N16 1.425(3) . ? C34 C35 1.393(4) . ? C34 H34A 0.9500 . ? C35 C36 1.381(4) . ? C35 N18 1.432(3) . ? C36 H36A 0.9500 . ? C37 N13 1.319(3) . ? C37 N14 1.364(3) . ? C37 H37A 0.9500 . ? C38 C39 1.336(4) . ? C38 N13 1.389(3) . ? C38 H38A 0.9500 . ? C39 N14 1.387(3) . ? C39 H39A 0.9500 . ? C40 N15 1.327(4) . ? C40 N16 1.355(4) . ? C40 H40A 0.9500 . ? C41 C42 1.346(4) . ? C41 N15 1.396(4) . ? C41 H41A 0.9500 . ? C42 N16 1.376(4) . ? C42 H42A 0.9500 . ? C43 N17 1.333(3) . ? C43 N18 1.336(3) . ? C43 H43A 0.9500 . ? C44 C45 1.358(4) . ? C44 N17 1.375(4) . ? C44 H44A 0.9500 . ? C45 N18 1.366(4) . ? C45 H45A 0.9500 . ? N3 Zn2 1.977(2) 2_646 ? N5 Zn2 2.004(2) 3_667 ? N9 Zn1 2.029(2) 3_567 ? N11 Zn1 2.240(2) 4_576 ? N17 Zn2 1.964(2) 2_646 ? O1 Cl1 1.437(3) . ? O2 Cl1 1.427(3) . ? O3 Cl1 1.423(3) . ? O4 Cl1 1.417(3) . ? O5 Cl2 1.446(8) . ? O6 Cl2 1.415(11) . ? O7 Cl2 1.408(11) . ? O8 Cl2 1.412(9) . ? O5A Cl2A 1.403(10) . ? O6A Cl2A 1.375(14) . ? O7A Cl2A 1.450(13) . ? O8A Cl2A 1.52(3) . ? O9 Cl3 1.421(4) . ? O10 Cl3 1.410(4) . ? O11 Cl3 1.445(3) . ? O12 Cl3 1.430(3) . ? O13 Cl4 1.407(3) . ? O14 Cl4 1.349(5) . ? O15 Cl4 1.274(5) . ? O16 Cl4 1.279(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Zn1 N9 122.23(9) . 3_567 ? N7 Zn1 N13 127.29(9) . . ? N9 Zn1 N13 110.46(9) 3_567 . ? N7 Zn1 N1 90.50(9) . . ? N9 Zn1 N1 90.85(9) 3_567 . ? N13 Zn1 N1 89.78(9) . . ? N7 Zn1 N11 89.97(9) . 4_575 ? N9 Zn1 N11 89.14(9) 3_567 4_575 ? N13 Zn1 N11 89.71(9) . 4_575 ? N1 Zn1 N11 179.45(9) . 4_575 ? N17 Zn2 N3 116.94(10) 2_656 2_656 ? N17 Zn2 N15 105.62(10) 2_656 . ? N3 Zn2 N15 114.62(10) 2_656 . ? N17 Zn2 N5 108.68(10) 2_656 3_667 ? N3 Zn2 N5 102.54(9) 2_656 3_667 ? N15 Zn2 N5 108.07(10) . 3_667 ? C2 C1 C6 122.6(2) . . ? C2 C1 N2 120.1(2) . . ? C6 C1 N2 117.3(2) . . ? C1 C2 C3 118.1(2) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C4 C3 C2 121.3(3) . . ? C4 C3 N4 118.8(2) . . ? C2 C3 N4 119.9(2) . . ? C5 C4 C3 118.1(2) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C4 C5 C6 122.3(3) . . ? C4 C5 N6 119.6(2) . . ? C6 C5 N6 118.1(2) . . ? C5 C6 C1 117.5(3) . . ? C5 C6 H6A 121.2 . . ? C1 C6 H6A 121.2 . . ? N1 C7 N2 110.8(2) . . ? N1 C7 H7A 124.6 . . ? N2 C7 H7A 124.6 . . ? C9 C8 N1 110.3(2) . . ? C9 C8 H8A 124.9 . . ? N1 C8 H8A 124.9 . . ? C8 C9 N2 106.0(2) . . ? C8 C9 H9A 127.0 . . ? N2 C9 H9A 127.0 . . ? N3 C10 N4 111.0(2) . . ? N3 C10 H10A 124.5 . . ? N4 C10 H10A 124.5 . . ? C12 C11 N3 109.2(2) . . ? C12 C11 H11A 125.4 . . ? N3 C11 H11A 125.4 . . ? C11 C12 N4 106.4(2) . . ? C11 C12 H12A 126.8 . . ? N4 C12 H12A 126.8 . . ? N5 C13 N6 110.5(2) . . ? N5 C13 H13A 124.7 . . ? N6 C13 H13A 124.7 . . ? C15 C14 N5 109.8(3) . . ? C15 C14 H14A 125.1 . . ? N5 C14 H14A 125.1 . . ? C14 C15 N6 105.5(3) . . ? C14 C15 H15A 127.3 . . ? N6 C15 H15A 127.3 . . ? C21 C16 C17 121.6(3) . . ? C21 C16 N8 118.2(2) . . ? C17 C16 N8 120.2(2) . . ? C18 C17 C16 118.7(2) . . ? C18 C17 H17A 120.6 . . ? C16 C17 H17A 120.6 . . ? C17 C18 C19 121.2(2) . . ? C17 C18 N10 120.0(2) . . ? C19 C18 N10 118.8(2) . . ? C20 C19 C18 118.6(3) . . ? C20 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? C19 C20 C21 122.3(3) . . ? C19 C20 N12 119.5(2) . . ? C21 C20 N12 118.1(2) . . ? C16 C21 C20 117.7(2) . . ? C16 C21 H21A 121.2 . . ? C20 C21 H21A 121.2 . . ? N7 C22 N8 110.4(2) . . ? N7 C22 H22A 124.8 . . ? N8 C22 H22A 124.8 . . ? C24 C23 N7 109.7(2) . . ? C24 C23 H23A 125.2 . . ? N7 C23 H23A 125.2 . . ? C23 C24 N8 106.6(2) . . ? C23 C24 H24A 126.7 . . ? N8 C24 H24A 126.7 . . ? N9 C25 N10 110.6(2) . . ? N9 C25 H25A 124.7 . . ? N10 C25 H25A 124.7 . . ? C27 C26 N9 109.5(2) . . ? C27 C26 H26A 125.3 . . ? N9 C26 H26A 125.3 . . ? C26 C27 N10 106.4(2) . . ? C26 C27 H27A 126.8 . . ? N10 C27 H27A 126.8 . . ? N11 C28 N12 110.9(2) . . ? N11 C28 H28A 124.5 . . ? N12 C28 H28A 124.5 . . ? C30 C29 N11 110.1(3) . . ? C30 C29 H29A 124.9 . . ? N11 C29 H29A 124.9 . . ? C29 C30 N12 106.0(3) . . ? C29 C30 H30A 127.0 . . ? N12 C30 H30A 127.0 . . ? C36 C31 C32 122.4(3) . . ? C36 C31 N14 119.0(2) . . ? C32 C31 N14 118.5(2) . . ? C31 C32 C33 117.3(2) . . ? C31 C32 H32A 121.3 . . ? C33 C32 H32A 121.3 . . ? C34 C33 C32 122.1(2) . . ? C34 C33 N16 118.3(2) . . ? C32 C33 N16 119.6(2) . . ? C33 C34 C35 117.9(3) . . ? C33 C34 H34A 121.0 . . ? C35 C34 H34A 121.0 . . ? C36 C35 C34 122.2(2) . . ? C36 C35 N18 119.7(2) . . ? C34 C35 N18 118.0(2) . . ? C35 C36 C31 118.0(2) . . ? C35 C36 H36A 121.0 . . ? C31 C36 H36A 121.0 . . ? N13 C37 N14 110.4(2) . . ? N13 C37 H37A 124.8 . . ? N14 C37 H37A 124.8 . . ? C39 C38 N13 110.1(2) . . ? C39 C38 H38A 124.9 . . ? N13 C38 H38A 124.9 . . ? C38 C39 N14 106.3(2) . . ? C38 C39 H39A 126.8 . . ? N14 C39 H39A 126.8 . . ? N15 C40 N16 109.9(2) . . ? N15 C40 H40A 125.1 . . ? N16 C40 H40A 125.1 . . ? C42 C41 N15 109.2(2) . . ? C42 C41 H41A 125.4 . . ? N15 C41 H41A 125.4 . . ? C41 C42 N16 106.4(3) . . ? C41 C42 H42A 126.8 . . ? N16 C42 H42A 126.8 . . ? N17 C43 N18 110.0(2) . . ? N17 C43 H43A 125.0 . . ? N18 C43 H43A 125.0 . . ? C45 C44 N17 108.8(3) . . ? C45 C44 H44A 125.6 . . ? N17 C44 H44A 125.6 . . ? C44 C45 N18 106.3(3) . . ? C44 C45 H45A 126.8 . . ? N18 C45 H45A 126.8 . . ? C7 N1 C8 105.4(2) . . ? C7 N1 Zn1 126.87(18) . . ? C8 N1 Zn1 127.65(18) . . ? C7 N2 C9 107.5(2) . . ? C7 N2 C1 125.7(2) . . ? C9 N2 C1 126.8(2) . . ? C10 N3 C11 106.0(2) . . ? C10 N3 Zn2 130.15(18) . 2_646 ? C11 N3 Zn2 122.28(18) . 2_646 ? C10 N4 C12 107.5(2) . . ? C10 N4 C3 126.5(2) . . ? C12 N4 C3 125.8(2) . . ? C13 N5 C14 106.7(2) . . ? C13 N5 Zn2 127.6(2) . 3_667 ? C14 N5 Zn2 124.68(19) . 3_667 ? C13 N6 C15 107.5(2) . . ? C13 N6 C5 125.6(2) . . ? C15 N6 C5 126.7(2) . . ? C22 N7 C23 105.6(2) . . ? C22 N7 Zn1 125.74(18) . . ? C23 N7 Zn1 128.35(18) . . ? C22 N8 C24 107.7(2) . . ? C22 N8 C16 126.4(2) . . ? C24 N8 C16 125.9(2) . . ? C25 N9 C26 106.3(2) . . ? C25 N9 Zn1 126.50(19) . 3_567 ? C26 N9 Zn1 127.10(18) . 3_567 ? C25 N10 C27 107.2(2) . . ? C25 N10 C18 126.1(2) . . ? C27 N10 C18 126.6(2) . . ? C28 N11 C29 105.7(2) . . ? C28 N11 Zn1 125.46(18) . 4_576 ? C29 N11 Zn1 127.55(19) . 4_576 ? C28 N12 C30 107.2(2) . . ? C28 N12 C20 126.5(2) . . ? C30 N12 C20 126.1(2) . . ? C37 N13 C38 106.0(2) . . ? C37 N13 Zn1 122.78(17) . . ? C38 N13 Zn1 131.17(18) . . ? C37 N14 C39 107.1(2) . . ? C37 N14 C31 125.0(2) . . ? C39 N14 C31 127.9(2) . . ? C40 N15 C41 106.3(2) . . ? C40 N15 Zn2 124.9(2) . . ? C41 N15 Zn2 128.22(18) . . ? C40 N16 C42 108.2(2) . . ? C40 N16 C33 123.3(2) . . ? C42 N16 C33 128.5(2) . . ? C43 N17 C44 106.4(2) . . ? C43 N17 Zn2 130.08(19) . 2_646 ? C44 N17 Zn2 123.42(19) . 2_646 ? C43 N18 C45 108.4(2) . . ? C43 N18 C35 124.7(2) . . ? C45 N18 C35 126.6(2) . . ? O7 Cl2 O8 112.6(8) . . ? O7 Cl2 O6 113.8(9) . . ? O8 Cl2 O6 110.1(7) . . ? O7 Cl2 O5 106.2(6) . . ? O8 Cl2 O5 111.0(7) . . ? O6 Cl2 O5 102.6(6) . . ? O6A Cl2A O5A 103.9(10) . . ? O6A Cl2A O7A 112.8(12) . . ? O5A Cl2A O7A 107.9(8) . . ? O6A Cl2A O8A 108.0(13) . . ? O5A Cl2A O8A 112.3(14) . . ? O7A Cl2A O8A 111.7(14) . . ? O4 Cl1 O3 108.77(18) . . ? O4 Cl1 O2 110.4(3) . . ? O3 Cl1 O2 109.1(2) . . ? O4 Cl1 O1 111.5(2) . . ? O3 Cl1 O1 110.54(19) . . ? O2 Cl1 O1 106.5(2) . . ? O10 Cl3 O9 110.8(3) . . ? O10 Cl3 O12 109.5(3) . . ? O9 Cl3 O12 110.4(2) . . ? O10 Cl3 O11 106.7(2) . . ? O9 Cl3 O11 109.1(2) . . ? O12 Cl3 O11 110.25(18) . . ? O15 Cl4 O16 106.5(8) . . ? O15 Cl4 O14 113.7(5) . . ? O16 Cl4 O14 98.0(6) . . ? O15 Cl4 O13 112.0(4) . . ? O16 Cl4 O13 115.7(6) . . ? O14 Cl4 O13 110.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.459 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 944999'