Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michael Scott' _publ_contact_author_address ; Department of Chemistry University of Florida P.O. Box 117200 Gainesville FL 32611 UNITED STATES OF AMERICA ; _publ_contact_author_email MJSCOTT@CHEM.UFL.EDU _publ_section_title ; Synthesis and Reactivity of a C3-Symmetric Trinuclear Zinc(II) Hydroxide Catalyst Efficient at Phosphate Diester Transesterification ; loop_ _publ_author_name 'Michael Scott' 'Ranjan Mitra' 'Matthew W. Peters' data_freeamineligand _database_code_depnum_ccdc_archive 'CCDC 645249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '5,free ligand' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H105 N9 O4' _chemical_formula_weight 1184.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 16.7988(5) _cell_length_b 16.7988(5) _cell_length_c 102.377(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25020.1(15) _cell_formula_units_Z 12 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7728 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type 'Corrected by Sadabs' _exptl_absorpt_correction_T_min 0.727010 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55786 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -134 _diffrn_reflns_limit_l_max 123 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.03 _reflns_number_total 6727 _reflns_number_gt 2885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart CCD' _computing_cell_refinement 'Smart CCD' _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELX XP' _computing_publication_material 'Microsoft Word' _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 contained a badly disordered THF solvate molecule and it was removed from the structure by the Squeeze from the Platon Program package. ; _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^)+(0.1376P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6727 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1716 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2630 _refine_ls_wR_factor_gt 0.2202 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 O1 O 0.46915(12) 0.67235(12) 0.075354(14) 0.0525(5) Uani 1 1 d . . . N1 N 0.56286(14) 0.77943(15) 0.100306(18) 0.0511(6) Uani 1 1 d . . . N2 N 0.55394(16) 0.72415(16) 0.12722(2) 0.0579(6) Uani 1 1 d . . . N3 N 0.5517(2) 0.5631(2) 0.15096(3) 0.0836(8) Uani 1 1 d . . . C1 C 0.3333 0.6667 0.05859(3) 0.0405(9) Uani 1 3 d S . . H1A H 0.3333 0.6667 0.0684 0.049 Uiso 1 3 calc SR . . C2 C 0.39614(16) 0.63007(16) 0.05432(2) 0.0420(6) Uani 1 1 d . . . C3 C 0.39090(18) 0.59169(18) 0.04216(2) 0.0493(6) Uani 1 1 d . . . H3A H 0.3449 0.5865 0.0363 0.059 Uiso 1 1 calc R . . C4 C 0.4489(2) 0.56069(19) 0.03817(2) 0.0547(7) Uani 1 1 d . . . C5 C 0.5125(2) 0.5646(2) 0.04731(3) 0.0606(8) Uani 1 1 d . . . H5A H 0.5520 0.5417 0.0449 0.073 Uiso 1 1 calc R . . C6 C 0.51996(19) 0.6008(2) 0.05973(3) 0.0589(7) Uani 1 1 d . . . C7 C 0.46302(17) 0.63579(18) 0.06302(2) 0.0484(6) Uani 1 1 d . . . C8 C 0.4449(2) 0.5275(2) 0.02411(3) 0.0693(9) Uani 1 1 d . . . C9 C 0.4762(3) 0.6139(3) 0.01491(3) 0.1187(16) Uani 1 1 d . . . H9A H 0.4745 0.5954 0.0058 0.178 Uiso 1 1 calc R . . H9B H 0.5390 0.6613 0.0172 0.178 Uiso 1 1 calc R . . H9C H 0.4346 0.6384 0.0161 0.178 Uiso 1 1 calc R . . C10 C 0.3503(3) 0.4616(3) 0.01994(4) 0.1241(18) Uani 1 1 d . . . H10A H 0.3261 0.4058 0.0253 0.186 Uiso 1 1 calc R . . H10B H 0.3505 0.4460 0.0107 0.186 Uiso 1 1 calc R . . H10C H 0.3114 0.4894 0.0211 0.186 Uiso 1 1 calc R . . C11 C 0.5160(4) 0.5010(4) 0.02135(4) 0.145(2) Uani 1 1 d . . . H11A H 0.5033 0.4472 0.0266 0.217 Uiso 1 1 calc R . . H11B H 0.5769 0.5523 0.0236 0.217 Uiso 1 1 calc R . . H11C H 0.5143 0.4861 0.0121 0.217 Uiso 1 1 calc R . . C12 C 0.5875(2) 0.6019(3) 0.06975(3) 0.0822(10) Uani 1 1 d . . . H12A H 0.6220 0.5749 0.0659 0.123 Uiso 1 1 calc R . . H12B H 0.5536 0.5660 0.0774 0.123 Uiso 1 1 calc R . . H12C H 0.6302 0.6654 0.0724 0.123 Uiso 1 1 calc R . . C13 C 0.53645(19) 0.7686(2) 0.07615(2) 0.0562(7) Uani 1 1 d . . . H13A H 0.5264 0.8020 0.0690 0.067 Uiso 1 1 calc R . . H13B H 0.5988 0.7769 0.0751 0.067 Uiso 1 1 calc R . . C14 C 0.5298(2) 0.8075(2) 0.08902(2) 0.0573(7) Uani 1 1 d . . . H14A H 0.5651 0.8754 0.0884 0.069 Uiso 1 1 calc R . . H14B H 0.4646 0.7893 0.0905 0.069 Uiso 1 1 calc R . . C15 C 0.49707(18) 0.68711(19) 0.10478(2) 0.0550(7) Uani 1 1 d . . . H15A H 0.4839 0.6429 0.0976 0.066 Uiso 1 1 calc R . . H15B H 0.4388 0.6847 0.1072 0.066 Uiso 1 1 calc R . . C16 C 0.5327(2) 0.6596(2) 0.11634(2) 0.0578(7) Uani 1 1 d . . . H16A H 0.4860 0.5970 0.1192 0.069 Uiso 1 1 calc R . . H16B H 0.5889 0.6582 0.1138 0.069 Uiso 1 1 calc R . . C17 C 0.5843(2) 0.8437(2) 0.11110(3) 0.0648(8) Uani 1 1 d . . . H17A H 0.5281 0.8450 0.1137 0.078 Uiso 1 1 calc R . . H17B H 0.6307 0.9063 0.1082 0.078 Uiso 1 1 calc R . . C18 C 0.6209(2) 0.8162(2) 0.12276(2) 0.0663(8) Uani 1 1 d . . . H18A H 0.6787 0.8177 0.1203 0.080 Uiso 1 1 calc R . . H18B H 0.6348 0.8607 0.1299 0.080 Uiso 1 1 calc R . . C19 C 0.5902(2) 0.6982(2) 0.13827(3) 0.0691(9) Uani 1 1 d . . . H19A H 0.6159 0.7492 0.1447 0.083 Uiso 1 1 calc R . . H19B H 0.6412 0.6893 0.1352 0.083 Uiso 1 1 calc R . . C20 C 0.5193(2) 0.6113(2) 0.14506(3) 0.0635(8) Uani 1 1 d . . . C21 C 0.4283(2) 0.5867(3) 0.14558(3) 0.0780(9) Uani 1 1 d . . . H21A H 0.4067 0.6227 0.1414 0.094 Uiso 1 1 calc R . . C22 C 0.3688(3) 0.5084(3) 0.15238(4) 0.0922(12) Uani 1 1 d . . . H22A H 0.3054 0.4897 0.1528 0.111 Uiso 1 1 calc R . . C23 C 0.4002(3) 0.4585(3) 0.15841(4) 0.0926(12) Uani 1 1 d . . . H23A H 0.3601 0.4047 0.1632 0.111 Uiso 1 1 calc R . . C24 C 0.4912(4) 0.4878(3) 0.15738(4) 0.1022(13) Uani 1 1 d . . . H24A H 0.5135 0.4522 0.1615 0.123 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0507(10) 0.0672(12) 0.0296(9) 0.0001(8) -0.0011(7) 0.0220(9) N1 0.0544(13) 0.0583(14) 0.0368(11) -0.0105(10) -0.0068(9) 0.0254(12) N2 0.0605(14) 0.0654(15) 0.0394(12) -0.0097(11) -0.0058(10) 0.0252(13) N3 0.085(2) 0.085(2) 0.0762(19) 0.0139(16) -0.0021(16) 0.0397(18) C1 0.0482(15) 0.0482(15) 0.0250(18) 0.000 0.000 0.0241(8) C2 0.0469(14) 0.0461(14) 0.0308(11) 0.0043(10) 0.0044(10) 0.0218(12) C3 0.0594(16) 0.0592(17) 0.0331(12) -0.0016(11) -0.0025(11) 0.0326(14) C4 0.0652(18) 0.0599(17) 0.0424(14) -0.0007(12) 0.0085(13) 0.0339(15) C5 0.0690(19) 0.073(2) 0.0529(16) 0.0046(14) 0.0083(14) 0.0457(16) C6 0.0600(18) 0.078(2) 0.0448(15) 0.0088(14) 0.0037(13) 0.0388(16) C7 0.0493(15) 0.0596(16) 0.0301(12) 0.0041(11) 0.0012(11) 0.0227(13) C8 0.076(2) 0.090(2) 0.0521(17) -0.0183(16) 0.0055(15) 0.0490(19) C9 0.164(4) 0.107(3) 0.0462(19) -0.0069(19) 0.012(2) 0.039(3) C10 0.091(3) 0.133(4) 0.089(3) -0.065(3) 0.016(2) 0.012(3) C11 0.162(5) 0.233(6) 0.073(2) -0.037(3) 0.010(3) 0.124(5) C12 0.081(2) 0.129(3) 0.0608(19) 0.0074(19) -0.0017(17) 0.071(2) C13 0.0526(16) 0.0682(19) 0.0390(14) 0.0003(13) -0.0027(11) 0.0236(15) C14 0.0575(17) 0.0653(18) 0.0517(16) -0.0016(13) -0.0007(13) 0.0326(15) C15 0.0523(16) 0.0624(18) 0.0392(14) -0.0071(12) -0.0037(12) 0.0204(14) C16 0.0598(17) 0.0625(18) 0.0432(14) -0.0083(13) -0.0022(12) 0.0248(15) C17 0.078(2) 0.0626(18) 0.0501(16) -0.0111(13) -0.0044(14) 0.0321(16) C18 0.075(2) 0.0621(19) 0.0433(15) -0.0148(13) -0.0103(14) 0.0202(16) C19 0.0608(18) 0.088(2) 0.0460(16) -0.0039(15) -0.0118(14) 0.0279(18) C20 0.0621(19) 0.075(2) 0.0394(14) -0.0088(14) -0.0025(13) 0.0237(17) C21 0.062(2) 0.098(3) 0.0604(18) -0.0018(18) 0.0029(16) 0.030(2) C22 0.069(2) 0.110(3) 0.068(2) -0.002(2) 0.0138(19) 0.022(2) C23 0.099(3) 0.085(3) 0.057(2) -0.0062(19) 0.009(2) 0.018(2) C24 0.128(4) 0.090(3) 0.078(2) 0.011(2) -0.001(3) 0.047(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 C7 1.386(3) . ? O1 C13 1.439(3) . ? N1 C15 1.457(3) . ? N1 C17 1.459(3) . ? N1 C14 1.459(3) . ? N2 C19 1.452(3) . ? N2 C18 1.458(4) . ? N2 C16 1.469(3) . ? N3 C20 1.324(4) . ? N3 C24 1.334(5) . ? C1 C2 1.527(3) 2_665 ? C1 C2 1.527(3) 3_565 ? C1 C2 1.527(3) . ? C2 C3 1.384(3) . ? C2 C7 1.398(3) . ? C3 C4 1.377(4) . ? C4 C5 1.397(4) . ? C4 C8 1.533(4) . ? C5 C6 1.388(4) . ? C6 C7 1.392(4) . ? C6 C12 1.522(4) . ? C8 C10 1.474(5) . ? C8 C11 1.496(5) . ? C8 C9 1.583(5) . ? C13 C14 1.500(4) . ? C15 C16 1.499(4) . ? C17 C18 1.516(4) . ? C19 C20 1.514(4) . ? C20 C21 1.372(4) . ? C21 C22 1.377(5) . ? C22 C23 1.343(6) . ? C23 C24 1.355(6) . ? 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 C7 O1 C13 113.08(18) . . ? C15 N1 C17 108.9(2) . . ? C15 N1 C14 112.6(2) . . ? C17 N1 C14 110.7(2) . . ? C19 N2 C18 110.2(2) . . ? C19 N2 C16 110.7(2) . . ? C18 N2 C16 108.6(2) . . ? C20 N3 C24 117.0(3) . . ? C2 C1 C2 112.15(14) 2_665 3_565 ? C2 C1 C2 112.15(14) 2_665 . ? C2 C1 C2 112.15(14) 3_565 . ? C3 C2 C7 117.8(2) . . ? C3 C2 C1 123.3(2) . . ? C7 C2 C1 118.9(2) . . ? C4 C3 C2 123.4(2) . . ? C3 C4 C5 117.0(2) . . ? C3 C4 C8 120.3(2) . . ? C5 C4 C8 122.7(2) . . ? C6 C5 C4 122.2(3) . . ? C5 C6 C7 118.4(2) . . ? C5 C6 C12 121.7(3) . . ? C7 C6 C12 119.8(2) . . ? O1 C7 C6 119.6(2) . . ? O1 C7 C2 119.3(2) . . ? C6 C7 C2 121.0(2) . . ? C10 C8 C11 116.3(3) . . ? C10 C8 C4 112.4(3) . . ? C11 C8 C4 112.9(3) . . ? C10 C8 C9 104.8(3) . . ? C11 C8 C9 102.2(3) . . ? C4 C8 C9 107.0(2) . . ? O1 C13 C14 110.6(2) . . ? N1 C14 C13 115.5(2) . . ? N1 C15 C16 111.7(2) . . ? N2 C16 C15 111.0(2) . . ? N1 C17 C18 111.0(2) . . ? N2 C18 C17 110.7(2) . . ? N2 C19 C20 113.6(2) . . ? N3 C20 C21 122.3(3) . . ? N3 C20 C19 115.7(3) . . ? C21 C20 C19 122.0(3) . . ? C20 C21 C22 118.3(4) . . ? C23 C22 C21 120.3(4) . . ? C22 C23 C24 117.4(4) . . ? N3 C24 C23 124.7(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.722 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.050 #===END data_Zn3OH3 _database_code_depnum_ccdc_archive 'CCDC 645250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 6,Zn3OH35 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H118 Cl3 N9 O21 Zn3' _chemical_formula_weight 1832.28 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 hexagonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 16.7532(16) _cell_length_b 16.7532(16) _cell_length_c 23.629(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5743.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type 'corrected by SADABS' _exptl_absorpt_correction_T_min 0.72113 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30250 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.50 _reflns_number_total 6406 _reflns_number_gt 3018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart CCD' _computing_cell_refinement 'Smart CCD' _computing_data_reduction Saint _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELX XP' _computing_publication_material 'Microsoft Word' _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 molecule crystallized with one perchlorate on the 3-fold position at full occupancy and the remaining perchlorate was disoreded on a general position with a site occupancy of 0.66666. There was also a severly disordered acetone molecule located on a general position and it was removed from the structure with SQUEEZE from the Platon Program Package. ; _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^)+(0.1627P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6406 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1436 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2616 _refine_ls_wR_factor_gt 0.2357 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 0.57999(5) 0.38151(5) 0.85671(3) 0.0635(3) Uani 1 1 d . . . O1 O 0.5441(3) 0.2538(3) 0.84693(17) 0.0677(12) Uani 1 1 d . . . H1B H 0.4820 0.2137 0.8359 0.081 Uiso 1 1 calc R . . O2 O 0.6123(3) 0.4353(3) 0.58174(15) 0.0689(12) Uani 1 1 d . . . N1 N 0.4916(4) 0.3773(4) 0.68935(19) 0.0617(13) Uani 1 1 d . . . N2 N 0.5235(4) 0.4454(4) 0.80422(19) 0.0671(15) Uani 1 1 d . . . N3 N 0.4996(4) 0.3979(4) 0.91594(19) 0.0669(15) Uani 1 1 d . . . C1 C 0.6667 0.3333 0.5099(4) 0.064(3) Uani 1 3 d S . . H1A H 0.6667 0.3333 0.5522 0.076 Uiso 1 3 calc SR . . C2 C 0.6724(4) 0.4225(5) 0.4914(2) 0.0621(17) Uani 1 1 d . . . C3 C 0.7088(5) 0.4621(5) 0.4390(2) 0.0675(18) Uani 1 1 d . . . H3A H 0.7326 0.4334 0.4151 0.081 Uiso 1 1 calc R . . C4 C 0.7115(5) 0.5419(6) 0.4205(3) 0.075(2) Uani 1 1 d . . . C5 C 0.6824(5) 0.5863(5) 0.4575(3) 0.080(2) Uani 1 1 d . . . H5A H 0.6867 0.6428 0.4464 0.096 Uiso 1 1 calc R . . C6 C 0.6468(5) 0.5497(5) 0.5108(3) 0.079(2) Uani 1 1 d . . . C7 C 0.6436(5) 0.4686(5) 0.5271(2) 0.0677(18) Uani 1 1 d . . . C8 C 0.7421(6) 0.5745(6) 0.3595(3) 0.093(3) Uani 1 1 d . . . C9 C 0.6730(7) 0.5044(6) 0.3186(3) 0.106(3) Uani 1 1 d . . . H9A H 0.6114 0.4943 0.3271 0.158 Uiso 1 1 calc R . . H9B H 0.6730 0.4462 0.3223 0.158 Uiso 1 1 calc R . . H9C H 0.6899 0.5275 0.2798 0.158 Uiso 1 1 calc R . . C10 C 0.7461(6) 0.6668(7) 0.3472(3) 0.120(3) Uani 1 1 d . . . H10A H 0.6838 0.6581 0.3493 0.180 Uiso 1 1 calc R . . H10B H 0.7715 0.6883 0.3093 0.180 Uiso 1 1 calc R . . H10C H 0.7855 0.7126 0.3754 0.180 Uiso 1 1 calc R . . C11 C 0.8374(7) 0.5846(8) 0.3465(4) 0.135(4) Uani 1 1 d . . . H11A H 0.8292 0.5246 0.3353 0.202 Uiso 1 1 calc R . . H11B H 0.8763 0.6068 0.3803 0.202 Uiso 1 1 calc R . . H11C H 0.8669 0.6287 0.3155 0.202 Uiso 1 1 calc R . . C12 C 0.6122(6) 0.5999(5) 0.5510(3) 0.097(3) Uani 1 1 d . . . H12A H 0.6426 0.6100 0.5879 0.145 Uiso 1 1 calc R . . H12B H 0.5453 0.5619 0.5559 0.145 Uiso 1 1 calc R . . H12C H 0.6269 0.6594 0.5345 0.145 Uiso 1 1 calc R . . C13 C 0.5136(5) 0.3722(5) 0.5863(2) 0.0726(19) Uani 1 1 d . . . H13A H 0.4927 0.3282 0.5542 0.087 Uiso 1 1 calc R . . H13B H 0.4805 0.4072 0.5843 0.087 Uiso 1 1 calc R . . C14 C 0.4920(5) 0.3207(5) 0.6407(2) 0.0688(18) Uani 1 1 d . . . H14A H 0.5383 0.3016 0.6478 0.083 Uiso 1 1 calc R . . H14B H 0.4308 0.2643 0.6378 0.083 Uiso 1 1 calc R . . C15 C 0.4390(4) 0.3187(5) 0.7360(2) 0.0660(17) Uani 1 1 d . . . H15A H 0.4696 0.2853 0.7504 0.079 Uiso 1 1 calc R . . H15B H 0.3767 0.2725 0.7226 0.079 Uiso 1 1 calc R . . C16 C 0.4309(5) 0.3752(5) 0.7829(3) 0.076(2) Uani 1 1 d . . . H16A H 0.3979 0.4064 0.7688 0.091 Uiso 1 1 calc R . . H16B H 0.3945 0.3340 0.8144 0.091 Uiso 1 1 calc R . . C17 C 0.5824(5) 0.4400(5) 0.7103(2) 0.0694(18) Uani 1 1 d . . . H17A H 0.6217 0.4783 0.6787 0.083 Uiso 1 1 calc R . . H17B H 0.6101 0.4045 0.7258 0.083 Uiso 1 1 calc R . . C18 C 0.5797(5) 0.5018(5) 0.7559(2) 0.0726(19) Uani 1 1 d . . . H18A H 0.6431 0.5453 0.7688 0.087 Uiso 1 1 calc R . . H18B H 0.5528 0.5381 0.7404 0.087 Uiso 1 1 calc R . . C19 C 0.5155(6) 0.5071(6) 0.8448(3) 0.085(2) Uani 1 1 d . . . H19A H 0.4766 0.5305 0.8285 0.102 Uiso 1 1 calc R . . H19B H 0.5773 0.5605 0.8525 0.102 Uiso 1 1 calc R . . C20 C 0.4733(5) 0.4570(5) 0.8990(3) 0.0718(19) Uani 1 1 d . . . C21 C 0.4128(6) 0.4708(6) 0.9302(3) 0.093(2) Uani 1 1 d . . . H21A H 0.3940 0.5128 0.9178 0.111 Uiso 1 1 calc R . . C22 C 0.3794(6) 0.4227(7) 0.9798(4) 0.098(3) Uani 1 1 d . . . H22A H 0.3389 0.4331 1.0027 0.117 Uiso 1 1 calc R . . C23 C 0.4040(5) 0.3605(6) 0.9962(3) 0.093(3) Uani 1 1 d . . . H23A H 0.3789 0.3254 1.0297 0.112 Uiso 1 1 calc R . . C24 C 0.4665(5) 0.3487(5) 0.9633(3) 0.0715(19) Uani 1 1 d . . . H24A H 0.4853 0.3061 0.9745 0.086 Uiso 1 1 calc R . . Cl1 Cl 0.6667 0.3333 1.01725(14) 0.0838(9) Uani 1 3 d S . . O3 O 0.6667 0.3333 0.9597(4) 0.153(5) Uani 1 3 d S . . O4 O 0.6947(5) 0.4213(4) 1.0389(3) 0.154(3) Uani 1 1 d . . . Cl2 Cl 0.3027(3) 0.1066(3) 0.87774(19) 0.1111(14) Uani 0.67 1 d P . . O5 O 0.3766(13) 0.1204(10) 0.8945(6) 0.207(6) Uani 0.67 1 d P . . O6 O 0.2138(9) 0.0627(10) 0.8739(6) 0.200(6) Uani 0.67 1 d P . . O7 O 0.3430(10) 0.1424(12) 0.8200(8) 0.158(6) Uani 0.50 1 d P . . O8 O 0.301(3) 0.197(3) 0.8939(18) 0.181(16) Uiso 0.25 1 d P . . O9 O 0.296(2) 0.029(3) 0.8571(13) 0.150(10) Uiso 0.25 1 d P . . O10 O 0.330(2) 0.182(2) 0.8642(15) 0.163(10) Uiso 0.33 1 d P . . 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 0.0774(6) 0.0828(6) 0.0361(4) -0.0083(3) -0.0057(3) 0.0443(5) O1 0.071(3) 0.083(3) 0.045(2) -0.007(2) -0.0011(19) 0.035(3) O2 0.086(3) 0.092(3) 0.034(2) -0.002(2) -0.008(2) 0.049(3) N1 0.072(4) 0.076(4) 0.040(3) -0.003(3) -0.001(2) 0.039(3) N2 0.092(4) 0.090(4) 0.035(3) -0.019(3) -0.011(3) 0.057(4) N3 0.074(4) 0.095(4) 0.031(3) -0.015(3) -0.004(2) 0.042(3) C1 0.077(5) 0.077(5) 0.038(6) 0.000 0.000 0.038(2) C2 0.069(4) 0.086(5) 0.030(3) -0.005(3) -0.007(3) 0.038(4) C3 0.088(5) 0.091(5) 0.036(3) 0.004(3) -0.006(3) 0.054(4) C4 0.076(5) 0.101(6) 0.052(4) 0.005(4) -0.014(3) 0.046(4) C5 0.106(6) 0.079(5) 0.055(4) 0.000(4) -0.022(4) 0.045(5) C6 0.091(5) 0.092(6) 0.055(4) -0.011(4) -0.020(4) 0.047(5) C7 0.081(5) 0.083(5) 0.035(3) -0.001(3) -0.011(3) 0.038(4) C8 0.111(7) 0.124(7) 0.055(4) 0.032(4) 0.001(4) 0.067(6) C9 0.159(8) 0.131(7) 0.043(4) -0.005(4) -0.027(5) 0.084(7) C10 0.123(7) 0.169(9) 0.063(5) 0.034(5) -0.008(5) 0.069(7) C11 0.127(8) 0.205(11) 0.089(6) 0.077(7) 0.024(6) 0.094(8) C12 0.143(8) 0.092(6) 0.064(5) -0.022(4) -0.018(5) 0.065(6) C13 0.098(6) 0.089(5) 0.038(4) -0.009(3) -0.009(3) 0.052(5) C14 0.087(5) 0.085(5) 0.041(3) -0.005(3) -0.004(3) 0.048(4) C15 0.068(4) 0.083(5) 0.044(3) 0.002(3) -0.007(3) 0.036(4) C16 0.085(5) 0.113(6) 0.043(4) 0.000(4) -0.001(3) 0.059(5) C17 0.080(5) 0.091(5) 0.034(3) -0.002(3) 0.000(3) 0.040(4) C18 0.097(5) 0.082(5) 0.046(4) 0.000(3) 0.000(3) 0.050(4) C19 0.120(6) 0.110(6) 0.057(4) 0.006(4) 0.001(4) 0.081(6) C20 0.097(5) 0.102(6) 0.041(4) -0.015(3) -0.009(3) 0.068(5) C21 0.123(7) 0.137(7) 0.053(4) -0.011(4) -0.004(4) 0.091(6) C22 0.110(7) 0.145(8) 0.073(5) -0.022(5) 0.001(5) 0.090(7) C23 0.081(6) 0.121(7) 0.053(4) -0.022(4) -0.006(4) 0.032(5) C24 0.077(5) 0.101(5) 0.045(4) -0.020(4) -0.013(3) 0.051(4) Cl1 0.0866(15) 0.0866(15) 0.078(2) 0.000 0.000 0.0433(8) O3 0.202(8) 0.202(8) 0.055(6) 0.000 0.000 0.101(4) O4 0.181(7) 0.093(4) 0.181(7) 0.009(4) 0.098(5) 0.062(5) Cl2 0.070(2) 0.082(3) 0.151(3) 0.060(2) -0.009(2) 0.0154(19) O5 0.220(16) 0.185(14) 0.181(14) 0.065(10) 0.014(12) 0.074(13) O6 0.111(10) 0.181(12) 0.267(16) 0.045(11) 0.072(10) 0.043(9) O7 0.128(11) 0.157(13) 0.171(15) 0.061(12) 0.052(10) 0.057(10) _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 O1 1.903(4) 3_665 ? Zn1 O1 1.925(4) . ? Zn1 N3 2.055(5) . ? Zn1 N2 2.143(5) . ? O1 Zn1 1.903(4) 2_655 ? O2 C7 1.401(7) . ? O2 C13 1.454(8) . ? N1 C17 1.437(8) . ? N1 C15 1.445(7) . ? N1 C14 1.491(7) . ? N2 C19 1.464(8) . ? N2 C18 1.481(8) . ? N2 C16 1.490(8) . ? N3 C20 1.329(8) . ? N3 C24 1.336(8) . ? C1 C2 1.512(7) 3_665 ? C1 C2 1.512(7) 2_655 ? C1 C2 1.512(7) . ? C2 C7 1.382(9) . ? C2 C3 1.394(8) . ? C3 C4 1.385(9) . ? C4 C5 1.385(10) . ? C4 C8 1.537(9) . ? C5 C6 1.398(9) . ? C6 C7 1.388(9) . ? C6 C12 1.559(10) . ? C8 C9 1.514(11) . ? C8 C10 1.541(12) . ? C8 C11 1.549(11) . ? C13 C14 1.490(8) . ? C15 C16 1.508(9) . ? C17 C18 1.509(8) . ? C19 C20 1.501(10) . ? C20 C21 1.363(9) . ? C21 C22 1.373(11) . ? C22 C23 1.354(11) . ? C23 C24 1.396(10) . ? Cl1 O3 1.359(10) . ? Cl1 O4 1.401(6) 3_665 ? Cl1 O4 1.401(7) 2_655 ? Cl1 O4 1.401(6) . ? Cl2 O10 1.16(3) . ? Cl2 O5 1.208(18) . ? Cl2 O6 1.292(13) . ? Cl2 O9 1.35(4) . ? Cl2 O7 1.508(16) . ? Cl2 O8 1.57(4) . ? O5 O9 1.70(4) . ? O5 O10 1.74(3) . ? O6 O9 1.78(3) . ? O7 O10 1.32(3) . ? O8 O10 0.95(4) . ? 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 Zn1 O1 109.4(2) 3_665 . ? O1 Zn1 N3 127.28(19) 3_665 . ? O1 Zn1 N3 111.7(2) . . ? O1 Zn1 N2 104.3(2) 3_665 . ? O1 Zn1 N2 121.01(19) . . ? N3 Zn1 N2 81.0(2) . . ? Zn1 O1 Zn1 127.6(2) 2_655 . ? C7 O2 C13 114.9(4) . . ? C17 N1 C15 107.3(5) . . ? C17 N1 C14 113.0(5) . . ? C15 N1 C14 110.5(5) . . ? C19 N2 C18 108.0(5) . . ? C19 N2 C16 110.6(6) . . ? C18 N2 C16 108.8(5) . . ? C19 N2 Zn1 101.1(4) . . ? C18 N2 Zn1 117.8(4) . . ? C16 N2 Zn1 110.3(4) . . ? C20 N3 C24 121.5(6) . . ? C20 N3 Zn1 112.2(4) . . ? C24 N3 Zn1 125.8(5) . . ? C2 C1 C2 112.0(4) 3_665 2_655 ? C2 C1 C2 112.0(4) 3_665 . ? C2 C1 C2 112.0(4) 2_655 . ? C7 C2 C3 117.9(6) . . ? C7 C2 C1 120.6(6) . . ? C3 C2 C1 121.5(6) . . ? C4 C3 C2 122.3(6) . . ? C5 C4 C3 118.0(6) . . ? C5 C4 C8 123.1(7) . . ? C3 C4 C8 118.8(7) . . ? C4 C5 C6 121.4(7) . . ? C7 C6 C5 118.5(7) . . ? C7 C6 C12 121.1(6) . . ? C5 C6 C12 120.4(7) . . ? C2 C7 C6 121.7(6) . . ? C2 C7 O2 120.4(6) . . ? C6 C7 O2 117.9(6) . . ? C9 C8 C4 109.5(7) . . ? C9 C8 C10 106.9(6) . . ? C4 C8 C10 111.8(7) . . ? C9 C8 C11 107.7(8) . . ? C4 C8 C11 111.6(6) . . ? C10 C8 C11 109.1(7) . . ? O2 C13 C14 110.1(5) . . ? C13 C14 N1 112.0(5) . . ? N1 C15 C16 110.5(6) . . ? N2 C16 C15 111.1(5) . . ? N1 C17 C18 111.3(6) . . ? N2 C18 C17 109.9(6) . . ? N2 C19 C20 110.3(6) . . ? N3 C20 C21 121.0(7) . . ? N3 C20 C19 115.8(6) . . ? C21 C20 C19 123.3(7) . . ? C20 C21 C22 118.8(8) . . ? C23 C22 C21 120.3(7) . . ? C22 C23 C24 119.2(8) . . ? N3 C24 C23 119.1(7) . . ? O3 Cl1 O4 111.4(3) . 3_665 ? O3 Cl1 O4 111.4(4) . 2_655 ? O4 Cl1 O4 107.4(4) 3_665 2_655 ? O3 Cl1 O4 111.4(4) . . ? O4 Cl1 O4 107.4(4) 3_665 . ? O4 Cl1 O4 107.4(4) 2_655 . ? O10 Cl2 O5 94.6(16) . . ? O10 Cl2 O6 108.1(17) . . ? O5 Cl2 O6 155.7(10) . . ? O10 Cl2 O9 140(2) . . ? O5 Cl2 O9 83.5(15) . . ? O6 Cl2 O9 84.6(15) . . ? O10 Cl2 O7 57.5(17) . . ? O5 Cl2 O7 90.4(9) . . ? O6 Cl2 O7 108.9(9) . . ? O9 Cl2 O7 82.1(16) . . ? O10 Cl2 O8 37(2) . . ? O5 Cl2 O8 104.3(17) . . ? O6 Cl2 O8 89.7(15) . . ? O9 Cl2 O8 171(2) . . ? O7 Cl2 O8 93.3(17) . . ? Cl2 O5 O9 51.7(13) . . ? Cl2 O5 O10 41.5(12) . . ? O9 O5 O10 86.1(18) . . ? Cl2 O6 O9 49.0(12) . . ? O10 O7 Cl2 47.7(15) . . ? O10 O8 Cl2 47(3) . . ? Cl2 O9 O5 44.8(12) . . ? Cl2 O9 O6 46.4(12) . . ? O5 O9 O6 89.2(19) . . ? O8 O10 Cl2 96(4) . . ? O8 O10 O7 163(5) . . ? Cl2 O10 O7 75(2) . . ? O8 O10 O5 107(4) . . ? Cl2 O10 O5 43.8(12) . . ? O7 O10 O5 77(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.612 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.094 #===END