# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Leigh Jones' 'Euan Brechin' 'Peter W. Dunne' 'Georgios Karotsis' 'P. McArdle' 'Cecelia McDonald' 'Sean Meally' 'Giannis Papaefstathiou' 'Nicholas P. Power' _publ_contact_author_name 'Leigh Jones' _publ_contact_author_email LEIGH.JONES@NUIGALWAY.IE _publ_section_title ; A Family of Double-Bowl Pseudo Metallocalix[6]arene Discs. ; # Attachment '[Ni7](2).cif' data_cmd15c-1 _database_code_depnum_ccdc_archive 'CCDC 758960' #TrackingRef '[Ni7](2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni7(OH)6(L1)6](NO3)2.2MeOH' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H66 N8 Ni7 O26' _chemical_formula_weight 1678.14 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 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, -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' _cell_length_a 13.913(2) _cell_length_b 13.913(2) _cell_length_c 23.141(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3879.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 1.736 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.75349 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 9319 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.9275 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0450344164 _diffrn_orient_matrix_UB_12 -0.0101448073 _diffrn_orient_matrix_UB_13 -0.0183856129 _diffrn_orient_matrix_UB_21 0.0380583696 _diffrn_orient_matrix_UB_22 0.0316719545 _diffrn_orient_matrix_UB_23 -0.0222021176 _diffrn_orient_matrix_UB_31 -0.0016105943 _diffrn_orient_matrix_UB_32 -0.0487255259 _diffrn_orient_matrix_UB_33 -0.0105994699 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -39.00 81.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 0.0000 90.0000 120 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2335 _reflns_number_gt 2034 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1510P)^2^+14.9009P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 2335 _refine_ls_number_parameters 153 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.2155 _refine_ls_wR_factor_gt 0.2101 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Ni1 Ni 0.0000 0.0000 0.0000 0.0208(4) Uani 1 6 d S . . Ni2 Ni 0.10125(6) -0.15384(6) 0.00750(3) 0.0271(3) Uani 1 1 d . . . O1 O 0.1241(3) -0.0109(3) 0.04403(16) 0.0243(8) Uani 1 1 d . . . H1 H 0.1295 -0.0024 0.0870 0.029 Uiso 1 1 calc R . . O2 O -0.0417(3) -0.2787(3) 0.03428(17) 0.0274(9) Uani 1 1 d . . . O3 O -0.2540(3) -0.3965(3) 0.0572(2) 0.0396(11) Uani 1 1 d . . . O4 O 0.3546(6) -0.2344(6) 0.2023(3) 0.087(2) Uani 1 1 d . . . O9 O 0.0000 -0.095(5) 0.2500 0.17(2) Uiso 0.33 2 d SPD . . O10 O 0.365(4) 0.056(4) 0.2871(18) 0.081(12) Uiso 0.17 1 d PD . . N1 N 0.1767(4) -0.2013(5) 0.0698(2) 0.0368(12) Uani 1 1 d . . . N2 N 0.3333 -0.3333 0.2021(5) 0.051(3) Uani 1 3 d S . . C1 C 0.2995(6) -0.1400(8) 0.0707(4) 0.064(2) Uani 1 1 d . . . H1A H 0.3257 -0.1622 0.1047 0.096 Uiso 1 1 calc R . . H1B H 0.3267 -0.0601 0.0723 0.096 Uiso 1 1 calc R . . H1C H 0.3274 -0.1572 0.0356 0.096 Uiso 1 1 calc R . . C2 C 0.1279(6) -0.2747(6) 0.1095(3) 0.0422(16) Uani 1 1 d . . . H2 H 0.1743 -0.2860 0.1355 0.051 Uiso 1 1 calc R . . C3 C 0.0101(6) -0.3416(5) 0.1184(3) 0.0366(14) Uani 1 1 d . . . C4 C -0.0661(5) -0.3389(5) 0.0823(2) 0.0291(12) Uani 1 1 d . . . C5 C -0.1815(6) -0.4082(5) 0.0957(3) 0.0379(15) Uani 1 1 d . . . C6 C -0.3581(6) -0.4938(6) 0.0458(4) 0.059(2) Uani 1 1 d . . . H6A H -0.3460 -0.5560 0.0374 0.089 Uiso 1 1 calc R . . H6B H -0.3933 -0.4805 0.0124 0.089 Uiso 1 1 calc R . . H6C H -0.4064 -0.5116 0.0796 0.089 Uiso 1 1 calc R . . C7 C -0.2153(6) -0.4738(6) 0.1433(3) 0.0487(18) Uani 1 1 d . . . H7 H -0.2921 -0.5181 0.1518 0.058 Uiso 1 1 calc R . . C8 C -0.1358(6) -0.4756(6) 0.1797(3) 0.0492(17) Uani 1 1 d . . . H8 H -0.1592 -0.5212 0.2132 0.059 Uiso 1 1 calc R . . C9 C -0.0258(6) -0.4130(6) 0.1678(3) 0.0469(17) Uani 1 1 d . . . H9 H 0.0271 -0.4167 0.1922 0.056 Uiso 1 1 calc R . . C20 C 0.3501(19) 0.0000 0.2500 0.035(6) Uiso 0.33 2 d SPD . . C21 C 0.0000 -0.194(3) 0.2500 0.076(11) Uiso 0.33 2 d SPD . . 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 Ni1 0.0188(5) 0.0188(5) 0.0248(8) 0.000 0.000 0.0094(3) Ni2 0.0234(5) 0.0238(5) 0.0355(5) 0.0065(3) 0.0054(3) 0.0128(3) O1 0.0213(19) 0.029(2) 0.0239(18) 0.0003(15) 0.0019(14) 0.0133(15) O2 0.0246(19) 0.024(2) 0.032(2) 0.0068(16) -0.0014(16) 0.0110(16) O3 0.026(2) 0.029(2) 0.054(3) 0.009(2) -0.0047(19) 0.0068(19) O4 0.091(5) 0.069(4) 0.098(5) -0.005(4) -0.033(4) 0.039(4) N1 0.029(3) 0.044(3) 0.043(3) 0.012(2) 0.002(2) 0.023(2) N2 0.057(4) 0.057(4) 0.040(6) 0.000 0.000 0.028(2) C1 0.037(4) 0.079(6) 0.078(6) 0.028(5) 0.002(4) 0.030(4) C2 0.047(4) 0.044(4) 0.040(4) 0.008(3) 0.000(3) 0.026(3) C3 0.040(3) 0.032(3) 0.038(3) -0.001(3) -0.005(3) 0.019(3) C4 0.038(3) 0.022(3) 0.028(3) -0.001(2) -0.002(2) 0.015(2) C5 0.043(4) 0.027(3) 0.041(4) 0.003(3) 0.004(3) 0.016(3) C6 0.032(4) 0.032(4) 0.095(7) -0.002(4) -0.008(4) 0.001(3) C7 0.041(4) 0.040(4) 0.048(4) 0.010(3) 0.004(3) 0.008(3) C8 0.051(4) 0.046(4) 0.043(4) 0.003(3) -0.005(3) 0.019(3) C9 0.052(4) 0.043(4) 0.038(4) 0.006(3) -0.004(3) 0.017(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 Ni1 O1 2.075(3) 7 ? Ni1 O1 2.075(3) 9 ? Ni1 O1 2.075(3) 8 ? Ni1 O1 2.075(3) 2 ? Ni1 O1 2.075(3) . ? Ni1 O1 2.075(3) 3 ? Ni2 O2 1.976(4) . ? Ni2 O2 1.998(4) 9 ? Ni2 O1 2.034(4) . ? Ni2 N1 2.077(5) . ? Ni2 O1 2.082(4) 8 ? Ni2 O3 2.306(4) 9 ? O1 Ni2 2.082(4) 9 ? O1 H1 1.0000 . ? O2 C4 1.328(7) . ? O2 Ni2 1.998(4) 8 ? O3 C5 1.415(8) . ? O3 C6 1.428(7) . ? O3 Ni2 2.306(4) 8 ? O4 N2 1.255(7) . ? O9 C21 1.38(7) . ? O10 C20 1.11(4) . ? N1 C2 1.286(8) . ? N1 C1 1.480(9) . ? N2 O4 1.255(7) 2_545 ? N2 O4 1.255(7) 3_655 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.439(10) . ? C2 H2 0.9500 . ? C3 C4 1.366(9) . ? C3 C9 1.430(9) . ? C4 C5 1.434(9) . ? C5 C7 1.355(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.401(11) . ? C7 H7 0.9500 . ? C8 C9 1.358(10) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C20 O10 1.11(4) 5 ? 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 Ni1 O1 97.96(13) 7 9 ? O1 Ni1 O1 97.96(13) 7 8 ? O1 Ni1 O1 97.96(13) 9 8 ? O1 Ni1 O1 82.04(13) 7 2 ? O1 Ni1 O1 82.04(13) 9 2 ? O1 Ni1 O1 180.0(3) 8 2 ? O1 Ni1 O1 180.0(3) 7 . ? O1 Ni1 O1 82.04(13) 9 . ? O1 Ni1 O1 82.04(13) 8 . ? O1 Ni1 O1 97.96(13) 2 . ? O1 Ni1 O1 82.04(13) 7 3 ? O1 Ni1 O1 180.00(18) 9 3 ? O1 Ni1 O1 82.04(13) 8 3 ? O1 Ni1 O1 97.96(13) 2 3 ? O1 Ni1 O1 97.96(13) . 3 ? O2 Ni2 O2 169.05(9) . 9 ? O2 Ni2 O1 109.04(16) . . ? O2 Ni2 O1 79.22(15) 9 . ? O2 Ni2 N1 87.07(19) . . ? O2 Ni2 N1 98.84(19) 9 . ? O1 Ni2 N1 99.51(19) . . ? O2 Ni2 O1 78.58(15) . 8 ? O2 Ni2 O1 95.76(16) 9 8 ? O1 Ni2 O1 82.9(2) . 8 ? N1 Ni2 O1 165.40(18) . 8 ? O2 Ni2 O3 96.75(16) . 9 ? O2 Ni2 O3 74.55(15) 9 9 ? O1 Ni2 O3 153.69(15) . 9 ? N1 Ni2 O3 86.6(2) . 9 ? O1 Ni2 O3 97.62(16) 8 9 ? Ni2 O1 Ni1 97.96(16) . . ? Ni2 O1 Ni2 98.36(15) . 9 ? Ni1 O1 Ni2 96.45(16) . 9 ? Ni2 O1 H1 119.7 . . ? Ni1 O1 H1 119.7 . . ? Ni2 O1 H1 119.7 9 . ? C4 O2 Ni2 130.1(4) . . ? C4 O2 Ni2 122.3(4) . 8 ? Ni2 O2 Ni2 103.23(17) . 8 ? C5 O3 C6 116.8(5) . . ? C5 O3 Ni2 110.2(3) . 8 ? C6 O3 Ni2 125.6(5) . 8 ? C2 N1 C1 116.6(6) . . ? C2 N1 Ni2 126.8(5) . . ? C1 N1 Ni2 116.6(4) . . ? O4 N2 O4 119.999(11) . 2_545 ? O4 N2 O4 119.999(12) . 3_655 ? O4 N2 O4 119.999(11) 2_545 3_655 ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 126.5(6) . . ? N1 C2 H2 116.8 . . ? C3 C2 H2 116.8 . . ? C4 C3 C9 120.1(6) . . ? C4 C3 C2 122.9(6) . . ? C9 C3 C2 117.0(6) . . ? O2 C4 C3 124.9(6) . . ? O2 C4 C5 116.9(5) . . ? C3 C4 C5 118.1(6) . . ? C7 C5 O3 124.1(6) . . ? C7 C5 C4 121.6(7) . . ? O3 C5 C4 114.1(5) . . ? O3 C6 H6A 109.5 . . ? O3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 C8 119.3(7) . . ? C5 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 120.9(7) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C3 119.9(7) . . ? C8 C9 H9 120.1 . . ? C3 C9 H9 120.1 . . ? O10 C20 O10 161(5) . 5 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.276 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.170 # Attachment '[Zn7](5).cif' data_sm3b-1 _database_code_depnum_ccdc_archive 'CCDC 758961' #TrackingRef '[Zn7](5).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn7(OH)6(L1)6](NO3)2.2MeOH.H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H66 N8 O27 Zn7' _chemical_formula_weight 1740.76 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 Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 13.902(2) _cell_length_b 13.902(2) _cell_length_c 23.353(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3908.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 2.187 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.75440 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 9140 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.0555 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0473368098 _diffrn_orient_matrix_UB_12 -0.0036238570 _diffrn_orient_matrix_UB_13 0.0081224808 _diffrn_orient_matrix_UB_21 0.0017993707 _diffrn_orient_matrix_UB_22 0.0256425698 _diffrn_orient_matrix_UB_23 0.0265809534 _diffrn_orient_matrix_UB_31 -0.0351781627 _diffrn_orient_matrix_UB_32 -0.0530147820 _diffrn_orient_matrix_UB_33 0.0122994421 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -43.00 77.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 0.0000 120.0000 120 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2361 _reflns_number_gt 1766 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1370P)^2^+1.0195P] 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 2361 _refine_ls_number_parameters 159 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.2107 _refine_ls_wR_factor_gt 0.1990 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.0000 0.0000 0.0000 0.0241(5) Uani 1 6 d S . . Zn2 Zn 0.10662(6) -0.15006(7) 0.01114(4) 0.0261(3) Uani 1 1 d . . . O1 O 0.1298(3) -0.0053(4) 0.0444(2) 0.0255(10) Uani 1 1 d . . . H1 H 0.1376 0.0071 0.0867 0.031 Uiso 1 1 calc R . . O2 O 0.2460(4) -0.0402(3) -0.03342(19) 0.0238(10) Uani 1 1 d . . . O3 O 0.1506(4) -0.2515(4) -0.0569(2) 0.0351(12) Uani 1 1 d . . . O4 O 0.4120(6) -0.2375(6) -0.2954(3) 0.068(2) Uani 1 1 d . . . O51 O 0.778(3) 0.123(3) -0.2206(14) 0.040(7) Uiso 0.17 1 d PD . . O56 O 0.073(4) 0.063(4) 0.156(2) 0.086(14) Uiso 0.17 1 d PD . . O57 O 0.186(2) 0.186(2) 0.2500 0.068(8) Uiso 0.33 2 d SP . . N1 N 0.3857(5) 0.1804(5) -0.0712(3) 0.0347(15) Uani 1 1 d . . . N2 N 0.3333 -0.3333 -0.2956(5) 0.042(3) Uani 1 3 d S . . C1 C 0.1386(8) -0.3587(7) -0.0505(4) 0.054(2) Uani 1 1 d . . . H1A H 0.0939 -0.4064 -0.0822 0.081 Uiso 1 1 calc R . . H1B H 0.1016 -0.3911 -0.0141 0.081 Uiso 1 1 calc R . . H1C H 0.2121 -0.3523 -0.0510 0.081 Uiso 1 1 calc R . . C2 C 0.2782(5) -0.0670(6) -0.0808(3) 0.0239(14) Uani 1 1 d . . . C3 C 0.2315(6) -0.1786(6) -0.0953(3) 0.0299(16) Uani 1 1 d . . . C4 C 0.2626(7) -0.2126(6) -0.1446(3) 0.0376(18) Uani 1 1 d . . . H4 H 0.2294 -0.2894 -0.1534 0.045 Uiso 1 1 calc R . . C5 C 0.3415(7) -0.1350(6) -0.1806(3) 0.0392(19) Uani 1 1 d . . . H5 H 0.3632 -0.1587 -0.2138 0.047 Uiso 1 1 calc R . . C6 C 0.3891(7) -0.0242(7) -0.1691(3) 0.0394(19) Uani 1 1 d . . . H6 H 0.4424 0.0289 -0.1946 0.047 Uiso 1 1 calc R . . C7 C 0.3582(6) 0.0114(6) -0.1184(3) 0.0306(16) Uani 1 1 d . . . C8 C 0.4098(6) 0.1301(6) -0.1104(3) 0.0360(18) Uani 1 1 d . . . H8 H 0.4670 0.1757 -0.1365 0.043 Uiso 1 1 calc R . . C9 C 0.4474(9) 0.3041(7) -0.0732(5) 0.066(3) Uani 1 1 d . . . H9A H 0.5059 0.3296 -0.1023 0.099 Uiso 1 1 calc R . . H9B H 0.4809 0.3335 -0.0357 0.099 Uiso 1 1 calc R . . H9C H 0.3959 0.3305 -0.0828 0.099 Uiso 1 1 calc R . . C54 C 0.664(2) 0.0000 -0.2500 0.035(7) Uiso 0.33 2 d SPD . . C55 C 0.144(4) 0.006(4) 0.166(2) 0.036(11) Uiso 0.17 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 0.0183(6) 0.0183(6) 0.0357(11) 0.000 0.000 0.0091(3) Zn2 0.0213(5) 0.0229(5) 0.0352(5) 0.0076(3) 0.0062(3) 0.0118(4) O1 0.022(2) 0.029(2) 0.028(2) -0.002(2) 0.000(2) 0.015(2) O2 0.022(2) 0.019(2) 0.030(3) 0.0012(19) 0.009(2) 0.0097(19) O3 0.043(3) 0.022(3) 0.047(3) 0.003(2) 0.011(3) 0.021(2) O4 0.069(5) 0.049(4) 0.078(5) -0.003(4) 0.028(4) 0.022(4) N1 0.027(3) 0.027(3) 0.043(4) 0.001(3) 0.017(3) 0.008(3) N2 0.047(4) 0.047(4) 0.030(6) 0.000 0.000 0.024(2) C1 0.056(6) 0.032(5) 0.078(7) 0.011(4) 0.010(5) 0.025(4) C2 0.024(3) 0.026(3) 0.027(3) -0.001(3) -0.001(3) 0.017(3) C3 0.032(4) 0.032(4) 0.033(4) 0.001(3) 0.001(3) 0.022(3) C4 0.053(5) 0.033(4) 0.034(4) -0.007(3) -0.007(4) 0.026(4) C5 0.054(5) 0.042(5) 0.025(4) -0.002(3) 0.006(4) 0.026(4) C6 0.052(5) 0.045(5) 0.030(4) 0.010(4) 0.010(4) 0.031(4) C7 0.033(4) 0.035(4) 0.028(4) 0.002(3) 0.001(3) 0.020(3) C8 0.032(4) 0.039(4) 0.032(4) 0.004(3) 0.009(3) 0.014(4) C9 0.073(7) 0.032(5) 0.071(7) -0.004(5) 0.039(6) 0.010(5) _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 2.114(4) 7 ? Zn1 O1 2.114(4) 9 ? Zn1 O1 2.114(4) . ? Zn1 O1 2.114(4) 2 ? Zn1 O1 2.114(4) 8 ? Zn1 O1 2.114(4) 3 ? Zn1 Zn2 3.1160(9) 7 ? Zn1 Zn2 3.1160(9) 2 ? Zn1 Zn2 3.1160(9) 3 ? Zn1 Zn2 3.1160(9) 9 ? Zn1 Zn2 3.1160(9) 8 ? Zn1 Zn2 3.1160(9) . ? Zn2 O1 2.027(4) . ? Zn2 O2 2.039(4) 8 ? Zn2 O2 2.052(4) . ? Zn2 N1 2.097(6) 8 ? Zn2 O1 2.115(4) 8 ? Zn2 O3 2.398(5) . ? Zn2 Zn2 3.1484(9) 9 ? Zn2 Zn2 3.1484(9) 8 ? O1 Zn2 2.115(4) 9 ? O1 H1 1.0000 . ? O2 C2 1.316(8) . ? O2 Zn2 2.039(4) 9 ? O3 C3 1.398(9) . ? O3 C1 1.422(8) . ? O4 N2 1.230(7) . ? O51 C54 1.79(3) . ? O56 C55 1.57(6) . ? O56 O56 1.65(8) 2 ? O56 O56 1.65(8) 3 ? O56 C55 1.88(7) 2 ? N1 C8 1.293(9) . ? N1 C9 1.490(10) . ? N1 Zn2 2.097(6) 9 ? N2 O4 1.230(7) 2_545 ? N2 O4 1.230(7) 3_655 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.391(10) . ? C2 C7 1.408(10) . ? C3 C4 1.394(10) . ? C4 C5 1.374(11) . ? C4 H4 0.9500 . ? C5 C6 1.365(11) . ? C5 H5 0.9500 . ? C6 C7 1.429(10) . ? C6 H6 0.9500 . ? C7 C8 1.446(10) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C54 O51 1.79(3) 4_554 ? C55 O56 1.88(7) 3 ? 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 97.98(16) 7 9 ? O1 Zn1 O1 180.0(3) 7 . ? O1 Zn1 O1 82.02(16) 9 . ? O1 Zn1 O1 82.02(16) 7 2 ? O1 Zn1 O1 82.02(16) 9 2 ? O1 Zn1 O1 97.98(16) . 2 ? O1 Zn1 O1 97.98(16) 7 8 ? O1 Zn1 O1 97.98(16) 9 8 ? O1 Zn1 O1 82.02(16) . 8 ? O1 Zn1 O1 180.0(3) 2 8 ? O1 Zn1 O1 82.02(16) 7 3 ? O1 Zn1 O1 180.0(2) 9 3 ? O1 Zn1 O1 97.98(16) . 3 ? O1 Zn1 O1 97.98(16) 2 3 ? O1 Zn1 O1 82.02(16) 8 3 ? O1 Zn1 Zn2 40.15(12) 7 7 ? O1 Zn1 Zn2 84.54(12) 9 7 ? O1 Zn1 Zn2 139.85(12) . 7 ? O1 Zn1 Zn2 42.56(12) 2 7 ? O1 Zn1 Zn2 137.44(12) 8 7 ? O1 Zn1 Zn2 95.46(12) 3 7 ? O1 Zn1 Zn2 95.46(12) 7 2 ? O1 Zn1 Zn2 42.56(12) 9 2 ? O1 Zn1 Zn2 84.54(12) . 2 ? O1 Zn1 Zn2 40.15(12) 2 2 ? O1 Zn1 Zn2 139.85(12) 8 2 ? O1 Zn1 Zn2 137.44(12) 3 2 ? Zn2 Zn1 Zn2 60.690(4) 7 2 ? O1 Zn1 Zn2 42.56(12) 7 3 ? O1 Zn1 Zn2 139.85(12) 9 3 ? O1 Zn1 Zn2 137.44(12) . 3 ? O1 Zn1 Zn2 84.54(12) 2 3 ? O1 Zn1 Zn2 95.46(12) 8 3 ? O1 Zn1 Zn2 40.15(12) 3 3 ? Zn2 Zn1 Zn2 60.690(4) 7 3 ? Zn2 Zn1 Zn2 119.310(4) 2 3 ? O1 Zn1 Zn2 137.44(12) 7 9 ? O1 Zn1 Zn2 40.15(12) 9 9 ? O1 Zn1 Zn2 42.56(12) . 9 ? O1 Zn1 Zn2 95.46(12) 2 9 ? O1 Zn1 Zn2 84.54(12) 8 9 ? O1 Zn1 Zn2 139.85(12) 3 9 ? Zn2 Zn1 Zn2 119.310(4) 7 9 ? Zn2 Zn1 Zn2 60.690(4) 2 9 ? Zn2 Zn1 Zn2 180.0 3 9 ? O1 Zn1 Zn2 84.54(12) 7 8 ? O1 Zn1 Zn2 137.44(12) 9 8 ? O1 Zn1 Zn2 95.46(12) . 8 ? O1 Zn1 Zn2 139.85(12) 2 8 ? O1 Zn1 Zn2 40.15(12) 8 8 ? O1 Zn1 Zn2 42.56(12) 3 8 ? Zn2 Zn1 Zn2 119.310(4) 7 8 ? Zn2 Zn1 Zn2 180.0 2 8 ? Zn2 Zn1 Zn2 60.690(4) 3 8 ? Zn2 Zn1 Zn2 119.310(4) 9 8 ? O1 Zn1 Zn2 139.85(12) 7 . ? O1 Zn1 Zn2 95.46(12) 9 . ? O1 Zn1 Zn2 40.15(12) . . ? O1 Zn1 Zn2 137.44(12) 2 . ? O1 Zn1 Zn2 42.56(12) 8 . ? O1 Zn1 Zn2 84.54(12) 3 . ? Zn2 Zn1 Zn2 180.00(4) 7 . ? Zn2 Zn1 Zn2 119.310(4) 2 . ? Zn2 Zn1 Zn2 119.310(4) 3 . ? Zn2 Zn1 Zn2 60.690(4) 9 . ? Zn2 Zn1 Zn2 60.690(4) 8 . ? O1 Zn2 O2 114.34(18) . 8 ? O1 Zn2 O2 80.42(18) . . ? O2 Zn2 O2 162.73(11) 8 . ? O1 Zn2 N1 104.1(2) . 8 ? O2 Zn2 N1 86.3(2) 8 8 ? O2 Zn2 N1 99.2(2) . 8 ? O1 Zn2 O1 84.1(2) . 8 ? O2 Zn2 O1 78.67(17) 8 8 ? O2 Zn2 O1 94.78(18) . 8 ? N1 Zn2 O1 164.8(2) 8 8 ? O1 Zn2 O3 151.32(17) . . ? O2 Zn2 O3 93.12(18) 8 . ? O2 Zn2 O3 71.22(17) . . ? N1 Zn2 O3 85.0(2) 8 . ? O1 Zn2 O3 93.90(18) 8 . ? O1 Zn2 Zn1 42.26(12) . . ? O2 Zn2 Zn1 93.01(12) 8 . ? O2 Zn2 Zn1 92.73(12) . . ? N1 Zn2 Zn1 141.68(19) 8 . ? O1 Zn2 Zn1 42.53(12) 8 . ? O3 Zn2 Zn1 133.23(13) . . ? O1 Zn2 Zn2 41.58(12) . 9 ? O2 Zn2 Zn2 152.01(12) 8 9 ? O2 Zn2 Zn2 39.52(12) . 9 ? N1 Zn2 Zn2 110.95(18) 8 9 ? O1 Zn2 Zn2 83.70(12) 8 9 ? O3 Zn2 Zn2 109.73(12) . 9 ? Zn1 Zn2 Zn2 59.655(2) . 9 ? O1 Zn2 Zn2 96.35(12) . 8 ? O2 Zn2 Zn2 39.84(12) 8 8 ? O2 Zn2 Zn2 133.86(14) . 8 ? N1 Zn2 Zn2 125.79(17) 8 8 ? O1 Zn2 Zn2 39.49(12) 8 8 ? O3 Zn2 Zn2 100.13(14) . 8 ? Zn1 Zn2 Zn2 59.655(2) . 8 ? Zn2 Zn2 Zn2 117.324(17) 9 8 ? Zn2 O1 Zn1 97.59(19) . . ? Zn2 O1 Zn2 98.93(18) . 9 ? Zn1 O1 Zn2 94.91(18) . 9 ? Zn2 O1 H1 120.0 . . ? Zn1 O1 H1 120.0 . . ? Zn2 O1 H1 120.0 9 . ? C2 O2 Zn2 129.3(4) . 9 ? C2 O2 Zn2 123.0(4) . . ? Zn2 O2 Zn2 100.64(18) 9 . ? C3 O3 C1 117.2(6) . . ? C3 O3 Zn2 110.3(4) . . ? C1 O3 Zn2 128.0(5) . . ? C55 O56 O56 130(4) . 2 ? C55 O56 O56 71(4) . 3 ? O56 O56 O56 60.000(4) 2 3 ? C55 O56 C55 163(5) . 2 ? O56 O56 C55 52(3) 2 2 ? O56 O56 C55 112(3) 3 2 ? C8 N1 C9 116.6(6) . . ? C8 N1 Zn2 126.8(5) . 9 ? C9 N1 Zn2 116.3(5) . 9 ? O4 N2 O4 119.999(13) 2_545 . ? O4 N2 O4 119.999(15) 2_545 3_655 ? O4 N2 O4 119.999(13) . 3_655 ? O3 C1 H1A 109.5 . . ? O3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 C3 119.0(6) . . ? O2 C2 C7 123.6(6) . . ? C3 C2 C7 117.4(6) . . ? C2 C3 C4 121.8(7) . . ? C2 C3 O3 114.3(6) . . ? C4 C3 O3 123.8(6) . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.8(7) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.6(7) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 120.4(7) . . ? C2 C7 C8 123.5(6) . . ? C6 C7 C8 116.0(7) . . ? N1 C8 C7 126.4(7) . . ? N1 C8 H8 116.8 . . ? C7 C8 H8 116.8 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O51 C54 O51 132(3) . 4_554 ? O56 C55 O56 56(3) . 3 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.805 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.158 # Attachment '[Zn7](6).cif' data_lfj60a-1 _database_code_depnum_ccdc_archive 'CCDC 758962' #TrackingRef '[Zn7](6).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn7(OH)6(immp)6](NO3)2.3MeNO2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H66 N11 O30 Zn7' _chemical_formula_weight 1842.80 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 Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 14.082(2) _cell_length_b 14.082(2) _cell_length_c 22.759(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3908.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1870 _exptl_absorpt_coefficient_mu 2.196 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.75109 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 9120 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.0275 _diffrn_reflns_theta_max 25.34 _diffrn_orient_matrix_UB_11 -0.0170553713 _diffrn_orient_matrix_UB_12 -0.0511294392 _diffrn_orient_matrix_UB_13 -0.0139947565 _diffrn_orient_matrix_UB_21 -0.0371105240 _diffrn_orient_matrix_UB_22 -0.0276363995 _diffrn_orient_matrix_UB_23 0.0233852042 _diffrn_orient_matrix_UB_31 -0.0416865513 _diffrn_orient_matrix_UB_32 0.0045481172 _diffrn_orient_matrix_UB_33 -0.0151191974 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 73.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 0.0000 -180.0000 122 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2338 _reflns_number_gt 2059 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1420P)^2^+11.7546P] 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 2338 _refine_ls_number_parameters 157 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2079 _refine_ls_wR_factor_gt 0.2035 _refine_ls_goodness_of_fit_ref 1.119 _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 Zn1 Zn 0.0000 0.0000 0.0000 0.0205(4) Uani 1 6 d S . . Zn2 Zn 0.25469(5) 0.14525(5) -0.01270(3) 0.0195(3) Uani 1 1 d . . . O1 O 0.1299(3) 0.1321(3) 0.04529(16) 0.0206(9) Uani 1 1 d . . . H1 H 0.1381 0.1267 0.0886 0.025 Uiso 1 1 calc R . . O2 O 0.2448(3) 0.2803(3) -0.03444(16) 0.0210(8) Uani 1 1 d . . . O3 O 0.1569(4) 0.4014(3) -0.05663(19) 0.0267(9) Uani 1 1 d . . . O4 O 0.4173(5) 0.6562(5) -0.2943(3) 0.0581(16) Uani 1 1 d . . . O5 O 0.097(3) 0.162(4) 0.1806(17) 0.29(2) Uiso 0.50 1 d PD . . O6 O -0.085(2) 0.085(3) 0.1728(11) 0.167(10) Uiso 0.50 1 d PD . . N1 N 0.3802(4) 0.1980(4) -0.0743(2) 0.0269(11) Uani 1 1 d . . . N2 N 0.3333 0.6667 -0.2948(4) 0.039(2) Uani 1 3 d S . . N3 N 0.005(3) 0.144(2) 0.1949(9) 0.165(14) Uiso 0.50 1 d PD . . C1 C 0.4370(7) 0.1328(7) -0.0765(4) 0.047(2) Uani 1 1 d . . . H1A H 0.3853 0.0580 -0.0894 0.071 Uiso 1 1 calc R . . H1B H 0.4647 0.1307 -0.0373 0.071 Uiso 1 1 calc R . . H1C H 0.4984 0.1670 -0.1042 0.071 Uiso 1 1 calc R . . C2 C 0.4103(5) 0.2760(5) -0.1121(3) 0.0284(13) Uani 1 1 d . . . H2 H 0.4691 0.2892 -0.1375 0.034 Uiso 1 1 calc R . . C3 C 0.3623(5) 0.3454(5) -0.1192(2) 0.0222(12) Uani 1 1 d . . . C4 C 0.2812(5) 0.3426(4) -0.0813(2) 0.0179(11) Uani 1 1 d . . . C5 C 0.2376(5) 0.4111(5) -0.0947(3) 0.0226(12) Uani 1 1 d . . . C6 C 0.2720(6) 0.4798(5) -0.1433(3) 0.0295(13) Uani 1 1 d . . . H6 H 0.2399 0.5235 -0.1521 0.035 Uiso 1 1 calc R . . C7 C 0.3544(6) 0.4840(5) -0.1790(3) 0.0331(15) Uani 1 1 d . . . H7 H 0.3801 0.5328 -0.2116 0.040 Uiso 1 1 calc R . . C8 C 0.3986(6) 0.4187(5) -0.1677(3) 0.0296(14) Uani 1 1 d . . . H8 H 0.4543 0.4223 -0.1927 0.035 Uiso 1 1 calc R . . C9 C 0.1433(5) 0.4937(5) -0.0478(3) 0.0319(14) Uani 1 1 d . . . H9A H 0.2152 0.5593 -0.0419 0.048 Uiso 1 1 calc R . . H9B H 0.0976 0.4816 -0.0130 0.048 Uiso 1 1 calc R . . H9C H 0.1078 0.5039 -0.0823 0.048 Uiso 1 1 calc R . . C10 C 0.0000 0.195(2) 0.2500 0.143(10) Uiso 1 2 d SD . . 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 0.0138(5) 0.0138(5) 0.0338(9) 0.000 0.000 0.0069(3) Zn2 0.0152(4) 0.0160(4) 0.0277(5) 0.0047(2) 0.0021(2) 0.0081(3) O1 0.017(2) 0.0155(19) 0.0265(18) 0.0002(15) 0.0010(15) 0.0066(16) O2 0.019(2) 0.0173(19) 0.029(2) 0.0066(15) 0.0072(15) 0.0102(17) O3 0.027(2) 0.019(2) 0.038(2) 0.0072(17) 0.0106(19) 0.0143(18) O4 0.050(4) 0.062(4) 0.070(4) 0.022(3) 0.014(3) 0.034(3) N1 0.025(3) 0.026(3) 0.035(3) 0.007(2) 0.007(2) 0.017(2) N2 0.041(4) 0.041(4) 0.033(5) 0.000 0.000 0.0207(19) C1 0.053(5) 0.051(5) 0.061(5) 0.022(4) 0.028(4) 0.044(4) C2 0.026(3) 0.030(3) 0.030(3) 0.005(3) 0.008(2) 0.015(3) C3 0.024(3) 0.015(3) 0.026(3) 0.000(2) 0.004(2) 0.008(2) C4 0.015(3) 0.013(2) 0.021(3) 0.000(2) 0.001(2) 0.004(2) C5 0.018(3) 0.016(3) 0.030(3) -0.003(2) 0.000(2) 0.007(2) C6 0.042(4) 0.020(3) 0.029(3) 0.002(2) -0.003(3) 0.017(3) C7 0.047(4) 0.027(3) 0.025(3) 0.006(2) 0.005(3) 0.018(3) C8 0.039(4) 0.026(3) 0.022(3) 0.003(2) 0.007(2) 0.014(3) C9 0.023(3) 0.021(3) 0.054(4) -0.002(3) 0.004(3) 0.012(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 O1 2.113(4) . ? Zn1 O1 2.113(4) 7 ? Zn1 O1 2.113(4) 3 ? Zn1 O1 2.113(4) 8 ? Zn1 O1 2.113(4) 9 ? Zn1 O1 2.113(4) 2 ? Zn1 Zn2 3.1296(8) 9 ? Zn1 Zn2 3.1296(8) 3 ? Zn1 Zn2 3.1296(8) 7 ? Zn1 Zn2 3.1296(7) 8 ? Zn1 Zn2 3.1296(8) 2 ? Zn2 O1 2.028(4) 8 ? Zn2 O2 2.036(4) . ? Zn2 O2 2.056(4) 8 ? Zn2 N1 2.080(5) . ? Zn2 O1 2.130(4) . ? Zn2 O3 2.413(4) 8 ? O1 Zn2 2.028(4) 9 ? O1 H1 1.0000 . ? O2 C4 1.311(6) . ? O2 Zn2 2.056(4) 9 ? O3 C5 1.379(7) . ? O3 C9 1.420(7) . ? O3 Zn2 2.413(4) 9 ? O4 N2 1.263(6) . ? O5 N3 1.224(18) . ? O6 N3 1.222(18) . ? N1 C2 1.289(8) . ? N1 C1 1.490(8) . ? N2 O4 1.263(6) 2_665 ? N2 O4 1.263(6) 3_565 ? N3 C10 1.470(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.448(8) . ? C2 H2 0.9500 . ? C3 C4 1.415(8) . ? C3 C8 1.421(8) . ? C4 C5 1.412(8) . ? C5 C6 1.387(8) . ? C6 C7 1.393(10) . ? C6 H6 0.9500 . ? C7 C8 1.369(10) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N3 1.470(18) 5 ? 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 180.00(17) . 7 ? O1 Zn1 O1 98.23(13) . 3 ? O1 Zn1 O1 81.77(13) 7 3 ? O1 Zn1 O1 81.77(13) . 8 ? O1 Zn1 O1 98.23(13) 7 8 ? O1 Zn1 O1 81.77(13) 3 8 ? O1 Zn1 O1 81.77(13) . 9 ? O1 Zn1 O1 98.23(13) 7 9 ? O1 Zn1 O1 180.0(2) 3 9 ? O1 Zn1 O1 98.23(13) 8 9 ? O1 Zn1 O1 98.23(13) . 2 ? O1 Zn1 O1 81.77(13) 7 2 ? O1 Zn1 O1 98.23(13) 3 2 ? O1 Zn1 O1 180.0(3) 8 2 ? O1 Zn1 O1 81.77(13) 9 2 ? O1 Zn1 Zn2 39.90(10) . 9 ? O1 Zn1 Zn2 140.10(10) 7 9 ? O1 Zn1 Zn2 137.32(10) 3 9 ? O1 Zn1 Zn2 95.92(10) 8 9 ? O1 Zn1 Zn2 42.68(10) 9 9 ? O1 Zn1 Zn2 84.08(10) 2 9 ? O1 Zn1 Zn2 140.10(10) . 3 ? O1 Zn1 Zn2 39.90(10) 7 3 ? O1 Zn1 Zn2 42.68(10) 3 3 ? O1 Zn1 Zn2 84.08(10) 8 3 ? O1 Zn1 Zn2 137.32(10) 9 3 ? O1 Zn1 Zn2 95.92(10) 2 3 ? Zn2 Zn1 Zn2 180.00(2) 9 3 ? O1 Zn1 Zn2 137.32(10) . 7 ? O1 Zn1 Zn2 42.68(10) 7 7 ? O1 Zn1 Zn2 84.08(10) 3 7 ? O1 Zn1 Zn2 140.10(10) 8 7 ? O1 Zn1 Zn2 95.92(10) 9 7 ? O1 Zn1 Zn2 39.90(10) 2 7 ? Zn2 Zn1 Zn2 119.157(4) 9 7 ? Zn2 Zn1 Zn2 60.843(4) 3 7 ? O1 Zn1 Zn2 84.08(10) . 8 ? O1 Zn1 Zn2 95.92(10) 7 8 ? O1 Zn1 Zn2 39.90(10) 3 8 ? O1 Zn1 Zn2 42.68(10) 8 8 ? O1 Zn1 Zn2 140.10(10) 9 8 ? O1 Zn1 Zn2 137.32(10) 2 8 ? Zn2 Zn1 Zn2 119.157(4) 9 8 ? Zn2 Zn1 Zn2 60.843(4) 3 8 ? Zn2 Zn1 Zn2 119.157(4) 7 8 ? O1 Zn1 Zn2 95.92(10) . 2 ? O1 Zn1 Zn2 84.08(10) 7 2 ? O1 Zn1 Zn2 140.10(10) 3 2 ? O1 Zn1 Zn2 137.32(10) 8 2 ? O1 Zn1 Zn2 39.90(10) 9 2 ? O1 Zn1 Zn2 42.68(10) 2 2 ? Zn2 Zn1 Zn2 60.843(4) 9 2 ? Zn2 Zn1 Zn2 119.157(4) 3 2 ? Zn2 Zn1 Zn2 60.843(4) 7 2 ? Zn2 Zn1 Zn2 180.000(12) 8 2 ? O1 Zn2 O2 114.68(16) 8 . ? O1 Zn2 O2 79.99(15) 8 8 ? O2 Zn2 O2 161.53(9) . 8 ? O1 Zn2 N1 104.91(18) 8 . ? O2 Zn2 N1 86.85(18) . . ? O2 Zn2 N1 100.55(19) 8 . ? O1 Zn2 O1 83.4(2) 8 . ? O2 Zn2 O1 78.08(15) . . ? O2 Zn2 O1 93.35(15) 8 . ? N1 Zn2 O1 164.82(18) . . ? O1 Zn2 O3 150.62(15) 8 8 ? O2 Zn2 O3 93.25(15) . 8 ? O2 Zn2 O3 70.89(15) 8 8 ? N1 Zn2 O3 84.60(19) . 8 ? O1 Zn2 O3 94.32(15) . 8 ? Zn2 O1 Zn1 98.15(16) 9 . ? Zn2 O1 Zn2 99.30(15) 9 . ? Zn1 O1 Zn2 95.04(15) . . ? Zn2 O1 H1 119.7 9 . ? Zn1 O1 H1 119.7 . . ? Zn2 O1 H1 119.7 . . ? C4 O2 Zn2 129.5(4) . . ? C4 O2 Zn2 124.0(4) . 9 ? Zn2 O2 Zn2 101.50(16) . 9 ? C5 O3 C9 118.6(5) . . ? C5 O3 Zn2 111.0(3) . 9 ? C9 O3 Zn2 125.7(4) . 9 ? C2 N1 C1 117.0(5) . . ? C2 N1 Zn2 127.8(4) . . ? C1 N1 Zn2 115.1(4) . . ? O4 N2 O4 119.99(2) 2_665 3_565 ? O4 N2 O4 119.99(2) 2_665 . ? O4 N2 O4 119.99(2) 3_565 . ? O6 N3 O5 131(3) . . ? O6 N3 C10 113(2) . . ? O5 N3 C10 115(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 125.7(6) . . ? N1 C2 H2 117.1 . . ? C3 C2 H2 117.1 . . ? C4 C3 C8 119.1(5) . . ? C4 C3 C2 123.7(5) . . ? C8 C3 C2 117.2(5) . . ? O2 C4 C5 118.3(5) . . ? O2 C4 C3 123.7(5) . . ? C5 C4 C3 118.0(5) . . ? O3 C5 C6 123.6(6) . . ? O3 C5 C4 114.5(5) . . ? C6 C5 C4 121.9(6) . . ? C5 C6 C7 119.3(6) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 120.6(6) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 121.0(6) . . ? C7 C8 H8 119.5 . . ? C3 C8 H8 119.5 . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 N3 118(2) . 5 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.249 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.207