Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _publ_contact_autor ; William T. A. Harrison Department of Chemistry, University of Aberdeen, Aberdeen, AB24 3UE, Scotland ; _publ_contact_author_phone '+44 (0)1224 272897' _publ_contact_author_fax '+44 (0)1224 272921' _publ_contact_author_email 'w.harrison@abdn.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _journal_coden_Cambridge 186 _publ_contact_letter ; Cif file to accompany submission B009641P ; loop_ _publ_author_name 'Harrison, William T. A.' 'MacLean, Elizabeth J.' 'Maxwell, Robert S.' 'Nenoff, Tina M.' 'Phillips, Mark L. F.' 'Teat, Simon J.' #============================================================================== data_gznco _database_code_CSD 154055 # # Hand edited by WTAH, 30 August 2000 # _audit_creation_date 00-04-27 _audit_creation_method CRYSTALS_ver_07-07-97 # EJM24b gZnBO Daresbury data #**************************************************************************** #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'decomposes before melting' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #**************************************************************************** _cell_length_a 9.0931(7) _cell_angle_alpha 90. _cell_length_b 9.0931(7) _cell_angle_beta 90. _cell_length_c 38.333(3) _cell_angle_gamma 90. _cell_volume 3169.5(4) _symmetry_cell_setting 'Tetragonal ' _symmetry_space_group_name_H-M 'P 41 21 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-y+1/2,x+1/2,z+1/4' '-x,-y,z+1/2' 'y+1/2,-x+1/2,z+3/4' '-x+1/2,y+1/2,-z+1/4' 'y,x,-z' 'x+1/2,-y+1/2,-z+3/4' '-y,-x,-z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Zn ' 0.2220 1.4310 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C6 H18 N9 O9 Zn1.50' _chemical_formula_moiety ' C6 H18 Zn1.50 O9 N9 ' _chemical_compound_source ; ; _chemical_formula_weight 458.33 _cell_measurement_reflns_used 25637 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 29.29 _cell_measurement_temperature 150(2) _cell_formula_units_Z 8 _exptl_crystal_description ' box ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.08 _exptl_crystal_density_diffrn 1.92 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1875.06 _exptl_absorpt_coefficient_mu 2.36 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8338 _exptl_absorpt_correction_T_max 0.8715 _exptl_absorpt_process_details 'SADABS' _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 31785 _reflns_number_total 4546 _diffrn_reflns_av_R_equivalents 0.035 _reflns_number_observed 4206 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 29.48 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 53 _reflns_observed_criterion >1.00\s(I) _refine_diff_density_min -0.78 _refine_diff_density_max 1.21 _refine_ls_number_reflns 4206 _refine_ls_number_parameters 236 _refine_ls_R_factor_obs 0.0305 _refine_ls_wR_factor_obs 0.0313 _refine_ls_goodness_of_fit_obs 1.0943 _refine_ls_shift/su_max 0.001573 _refine_ls_abs_structure_Flack '0.09(1)' _refine_ls_abs_structure_details 'Flack, 4546 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 0.861 0.271 0.657 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Zn1 0.738049(19) 0.738049(19) 0.0000 0.0107 1.0000 Uani Zn2 0.750845(15) 0.251631(14) -0.083727(4) 0.0109 1.0000 Uani C6 0.51973(15) 0.18208(16) -0.13126(4) 0.0129 1.0000 Uani C4 0.75007(16) 1.00606(15) -0.03610(4) 0.0126 1.0000 Uani C5 0.70308(16) 0.50802(16) -0.04712(4) 0.0124 1.0000 Uani O1 0.65221(12) 0.44284(11) -0.07511(3) 0.0143 1.0000 Uani O2 0.66144(11) 0.19856(12) -0.12832(3) 0.0161 1.0000 Uani O3 0.46237(11) 0.23184(14) -0.15995(3) 0.0194 1.0000 Uani O4 0.69661(13) 1.13509(12) -0.04322(3) 0.0175 1.0000 Uani O5 0.64851(12) 0.63830(11) -0.04054(3) 0.0164 1.0000 Uani O6 0.69596(12) 0.94501(11) -0.00846(3) 0.0153 1.0000 Uani O7 0.44448(13) 0.11958(15) -0.10833(3) 0.0237 1.0000 Uani O8 0.84857(14) 0.94639(13) -0.05427(3) 0.0213 1.0000 Uani O9 0.79650(12) 0.44878(12) -0.02809(3) 0.0169 1.0000 Uani C1 0.7591(2) 0.97080(18) 0.12432(4) 0.0191 1.0000 Uani C2 0.99911(16) 0.2504(2) 0.03898(4) 0.0168 1.0000 Uani C3 1.2513(2) 0.49818(16) -0.04149(4) 0.0171 1.0000 Uani N1 0.90226(17) 0.99103(17) 0.12010(4) 0.0254 1.0000 Uani N2 0.68489(17) 0.89320(18) 0.10065(4) 0.0260 1.0000 Uani N3 0.68935(17) 1.02813(19) 0.15130(4) 0.0276 1.0000 Uani N4 1.0810(2) 0.19530(19) 0.06388(4) 0.0311 1.0000 Uani N5 0.9899(2) 0.39391(17) 0.03464(4) 0.0312 1.0000 Uani N6 0.9229(2) 0.1618(2) 0.01830(5) 0.0401 1.0000 Uani N7 1.10602(16) 0.49090(16) -0.04065(4) 0.0224 1.0000 Uani N8 1.32623(16) 0.42502(18) -0.06534(4) 0.0237 1.0000 Uani N9 1.32145(17) 0.58072(17) -0.01799(4) 0.0237 1.0000 Uani H11 0.95645 1.04597 0.13681 0.046(2) 1.0000 Uiso H12 0.95075 0.95056 0.10036 0.046(2) 1.0000 Uiso H21 0.73471 0.85168 0.08122 0.046(2) 1.0000 Uiso H22 0.58188 0.87960 0.10323 0.046(2) 1.0000 Uiso H31 0.74172 1.08485 0.16800 0.046(2) 1.0000 Uiso H32 0.58664 1.01270 0.15399 0.046(2) 1.0000 Uiso H41 1.1345 0.25909 0.07885 0.046(2) 1.0000 Uiso H42 1.0871 0.09181 0.06694 0.046(2) 1.0000 Uiso H51 1.0444 0.45793 0.04936 0.046(2) 1.0000 Uiso H52 0.9291 0.43334 0.01679 0.046(2) 1.0000 Uiso H61 0.9273 0.0583 0.02140 0.046(2) 1.0000 Uiso H62 0.8635 0.2024 0.00032 0.046(2) 1.0000 Uiso H71 1.05271 0.54410 -0.02348 0.046(2) 1.0000 Uiso H72 1.05503 0.43218 -0.05720 0.046(2) 1.0000 Uiso H81 1.43055 0.43043 -0.06584 0.046(2) 1.0000 Uiso H82 1.27554 0.36653 -0.08198 0.046(2) 1.0000 Uiso H91 1.42572 0.58718 -0.01833 0.046(2) 1.0000 Uiso H92 1.26686 0.63306 -0.00089 0.046(2) 1.0000 Uiso 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 0.01081(7) 0.01081(7) 0.01059(12) 0.00064(5) -0.00064(5) 0.00022(8) Zn2 0.00995(9) 0.01220(9) 0.01066(11) 0.00090(5) 0.00001(4) 0.00086(7) C6 0.0125(6) 0.0114(6) 0.0147(6) -0.0029(5) 0.0007(5) 0.0007(5) C4 0.0120(6) 0.0137(6) 0.0122(6) -0.0014(5) -0.0031(5) -0.0018(5) C5 0.0112(6) 0.0135(6) 0.0124(6) 0.0020(5) 0.0039(5) -0.0024(4) O1 0.0162(5) 0.0147(5) 0.0120(5) -0.0020(4) -0.0037(4) 0.0014(4) O2 0.0115(4) 0.0232(5) 0.0134(4) -0.0048(4) -0.0006(4) -0.0005(4) O3 0.0128(4) 0.0301(6) 0.0152(5) 0.0019(4) -0.0013(4) 0.0007(4) O4 0.0228(6) 0.0141(5) 0.0155(5) 0.0034(4) 0.0041(4) 0.0036(4) O5 0.0192(5) 0.0139(5) 0.0161(4) -0.0033(4) -0.0026(4) 0.0029(4) O6 0.0188(5) 0.0130(4) 0.0139(5) 0.0024(4) 0.0037(4) 0.0013(4) O7 0.0158(5) 0.0296(7) 0.0257(6) 0.0113(5) 0.0042(4) 0.0017(5) O8 0.0240(6) 0.0198(5) 0.0199(5) 0.0006(4) 0.0086(4) 0.0036(4) O9 0.0149(5) 0.0187(5) 0.0171(5) 0.0012(4) -0.0030(4) -0.0000(4) C1 0.0204(8) 0.0211(6) 0.0160(7) -0.0020(5) -0.0020(5) -0.0001(6) C2 0.0170(6) 0.0144(7) 0.0190(7) -0.0033(5) -0.0021(5) 0.0012(5) C3 0.0161(7) 0.0200(7) 0.0153(7) -0.0015(6) -0.0009(5) -0.0003(5) N1 0.0177(7) 0.0355(8) 0.0230(7) -0.0101(6) -0.0002(5) -0.0028(6) N2 0.0225(7) 0.0297(8) 0.0258(7) -0.0124(6) -0.0045(6) -0.0019(6) N3 0.0223(7) 0.0381(9) 0.0225(7) -0.0122(6) 0.0030(5) -0.0058(6) N4 0.0346(9) 0.0310(9) 0.0279(8) 0.0071(7) -0.0070(6) 0.0092(6) N5 0.0548(11) 0.0173(7) 0.0216(7) 0.0009(6) 0.0045(7) 0.0038(7) N6 0.0306(9) 0.041(1) 0.049(1) -0.0256(9) -0.0135(8) 0.0017(7) N7 0.0155(6) 0.0308(8) 0.0209(7) -0.0067(6) -0.0002(5) -0.0024(5) N8 0.0133(6) 0.0337(8) 0.0241(7) -0.0139(6) 0.0005(5) -0.0016(6) N9 0.0188(6) 0.0262(7) 0.0261(7) -0.0117(6) -0.0030(5) -0.0009(5) _refine_ls_extinction_coef 179.7(243) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . O5 . 1.975(1) yes Zn1 . O5 6_555 1.975(1) yes Zn1 . O6 . 1.948(1) yes Zn1 . O6 6_555 1.948(1) yes Zn2 . O1 . 1.984(1) yes Zn2 . O2 . 1.954(1) yes Zn2 . O3 7_554 1.944(1) yes Zn2 . O4 1_545 1.9436(11) yes C4 . O4 . 1.2990(17) yes C4 . O6 . 1.2935(17) yes C4 . O8 . 1.2576(18) yes C5 . O1 . 1.3102(17) yes C5 . O5 . 1.3089(18) yes C5 . O9 . 1.2426(19) yes C6 . O2 . 1.3021(17) yes C6 . O3 . 1.2986(18) yes C6 . O7 . 1.2505(19) yes C1 . N1 . 1.325(2) yes C1 . N2 . 1.333(2) yes C1 . N3 . 1.321(2) yes C2 . N4 . 1.310(2) yes C2 . N5 . 1.319(2) yes C2 . N6 . 1.325(2) yes C3 . N7 . 1.323(2) yes C3 . N8 . 1.320(2) yes C3 . N9 . 1.335(2) yes N1 . H11 . 0.950 no N1 . H12 . 0.950 no N2 . H21 . 0.950 no N2 . H22 . 0.950 no N3 . H31 . 0.950 no N3 . H32 . 0.950 no N4 . H41 . 0.950 no N4 . H42 . 0.950 no N5 . H51 . 0.950 no N5 . H52 . 0.950 no N6 . H61 . 0.950 no N6 . H62 . 0.950 no N7 . H71 . 0.950 no N7 . H72 . 0.950 no N8 . H81 . 0.950 no N8 . H82 . 0.950 no N9 . H91 . 0.950 no N9 . H92 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O5 . Zn1 . O5 6_555 103.92(6) yes O5 . Zn1 . O6 . 103.40(4) yes O5 6_555 Zn1 . O6 . 116.04(4) yes O5 . Zn1 . O6 6_555 116.04(4) yes O5 6_555 Zn1 . O6 6_555 103.40(4) yes O6 . Zn1 . O6 6_555 114.05(6) yes O1 . Zn2 . O2 . 100.02(4) yes O1 . Zn2 . O3 7_554 113.59(5) yes O2 . Zn2 . O3 7_554 108.76(5) yes O1 . Zn2 . O4 1_545 103.30(4) yes O2 . Zn2 . O4 1_545 117.31(5) yes O3 7_554 Zn2 . O4 1_545 113.12(5) yes O2 . C6 . O3 . 115.51(13) yes O2 . C6 . O7 . 122.21(14) yes O3 . C6 . O7 . 122.26(13) yes O4 . C4 . O6 . 114.66(13) yes O4 . C4 . O8 . 122.68(14) yes O6 . C4 . O8 . 122.64(13) yes O1 . C5 . O5 . 115.68(13) yes O1 . C5 . O9 . 121.75(13) yes O5 . C5 . O9 . 122.57(14) yes Zn2 . O1 . C5 . 111.91(9) yes Zn2 . O2 . C6 . 121.06(9) yes Zn2 7_454 O3 . C6 . 122.0(1) yes Zn2 1_565 O4 . C4 . 124.4(1) yes Zn1 . O5 . C5 . 114.3(1) yes Zn1 . O6 . C4 . 118.45(9) yes N1 . C1 . N2 . 119.21(16) yes N1 . C1 . N3 . 120.85(16) yes N2 . C1 . N3 . 119.94(17) yes N4 . C2 . N5 . 120.41(17) yes N4 . C2 . N6 . 120.05(19) yes N5 . C2 . N6 . 119.53(17) yes N7 . C3 . N8 . 120.47(15) yes N7 . C3 . N9 . 119.28(15) yes N8 . C3 . N9 . 120.25(18) yes C1 . N1 . H11 . 120.0(1) no C1 . N1 . H12 . 120.0(1) no H11 . N1 . H12 . 120.000 no C1 . N2 . H21 . 120.2(1) no C1 . N2 . H22 . 119.8(1) no H21 . N2 . H22 . 120.000 no C1 . N3 . H31 . 120.1(1) no C1 . N3 . H32 . 119.9(1) no H31 . N3 . H32 . 120.000 no C2 . N4 . H41 . 119.86(11) no C2 . N4 . H42 . 120.14(11) no H41 . N4 . H42 . 120.000 no C2 . N5 . H51 . 119.92(11) no C2 . N5 . H52 . 120.08(11) no H51 . N5 . H52 . 120.000 no C2 . N6 . H61 . 120.33(12) no C2 . N6 . H62 . 119.67(12) no H61 . N6 . H62 . 120.000 no C3 . N7 . H71 . 120.05(9) no C3 . N7 . H72 . 119.95(9) no H71 . N7 . H72 . 120.000 no C3 . N8 . H81 . 120.2(1) no C3 . N8 . H82 . 119.8(1) no H81 . N8 . H82 . 120.000 no C3 . N9 . H91 . 120.2(1) no C3 . N9 . H92 . 119.8(1) no H91 . N9 . H92 . 120.000 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H11 O1 . . 2_655 0.95 1.976 2.9229(19) 174.7 no N1 H12 O8 . . 6_555 0.95 1.996 2.865(2) 151.2 no N2 H21 O8 . . 6_555 0.95 2.185 2.997(2) 142.8 no N2 H22 O7 . . 2_555 0.95 2.424 3.218(2) 141.0 no N3 H31 O5 . . 2_655 0.95 2.013 2.9368(19) 163.7 no N3 H32 O7 . . 2_555 0.95 2.031 2.934(2) 158.1 no N4 H41 O7 . . 6_655 0.95 2.034 2.857(2) 143.9 no N4 H42 O3 . . 2_645 0.95 2.209 2.896(2) 128.4 no N5 H51 O4 . . 6_555 0.95 2.334 3.070(2) 134.0 no N5 H51 O7 . . 6_655 0.95 2.365 3.095(2) 133.4 no N5 H52 O9 . . . 0.95 2.106 3.021(2) 161.3 no N6 H61 O8 . . 6_545 0.94 2.292 3.172(2) 153.7 no N6 H62 O4 . . 1_545 0.95 2.337 3.139(2) 141.7 no N7 H71 O6 . . 6_555 0.95 2.089 3.0273(19) 169.1 no N7 H72 O3 . . 5_554 0.95 2.126 3.0650(19) 169.5 no N8 H81 O1 . . 1_655 0.95 2.050 2.9921(18) 171.2 no N8 H82 O2 . . 5_554 0.95 1.935 2.8587(19) 163.7 no N9 H91 O5 . . 1_655 0.95 2.246 3.1410(19) 156.7 no N9 H92 O4 . . 6_555 0.95 2.151 3.0802(19) 165.4 no # end of file