# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kim, Kimoon' _publ_contact_author_email kkim@postech.ac.kr loop_ _publ_author_name K.Kim H.Kim Y.Sun Y.Kim T.Kajiwara M.Yamashita data_pbcn1 _database_code_depnum_ccdc_archive 'CCDC 793419' #TrackingRef '- CCDC_793419.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cobalt(ii) formate DEF solvate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Co6 O24' _chemical_formula_weight 893.80 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.8839(4) _cell_length_b 18.2370(8) _cell_length_c 18.0818(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3259.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6498 _cell_measurement_theta_min 2.234 _cell_measurement_theta_max 28.240 _exptl_crystal_description hexagonal _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 3.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4598 _exptl_absorpt_correction_T_max 0.5791 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'SMART CCD' _diffrn_measurement_method Omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18254 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3922 _reflns_number_gt 2998 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material 'Diamond 3.1' _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 contributions of the disordered DEF molecules were removed from the diffraction data using the SQUEEZE routine of PLATON software (c.a. 287 e/u.c), and then final refinements were carried out. ; _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^)+(0.0513P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3922 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 Co1 Co 0.57822(4) 0.17890(2) 0.06090(2) 0.01349(12) Uani 1 1 d . . . Co2 Co 0.38762(4) 0.28329(2) -0.03512(2) 0.01494(12) Uani 1 1 d . . . Co3 Co 0.5000 0.18737(4) 0.2500 0.01698(15) Uani 1 2 d S . . Co4 Co 0.5000 0.0000 0.0000 0.01667(15) Uani 1 2 d S . . O1 O 0.4944(2) 0.18515(13) -0.04526(12) 0.0177(5) Uani 1 1 d . . . O2 O 0.5005(3) 0.07185(13) -0.09028(14) 0.0271(6) Uani 1 1 d . . . O3 O 0.7076(2) 0.00735(13) 0.00869(15) 0.0252(6) Uani 1 1 d . . . O4 O 0.7553(2) 0.12687(13) 0.02214(13) 0.0184(5) Uani 1 1 d . . . O5 O 0.4735(2) 0.08382(13) 0.08067(12) 0.0177(5) Uani 1 1 d . . . O6 O 0.3897(2) 0.10832(15) 0.19332(14) 0.0268(6) Uani 1 1 d . . . O7 O 0.6537(2) 0.18636(13) 0.16832(12) 0.0181(5) Uani 1 1 d . . . O8 O 0.6981(2) 0.26963(12) 0.03194(12) 0.0174(5) Uani 1 1 d . . . O9 O 0.5575(2) 0.34708(13) -0.02570(14) 0.0230(5) Uani 1 1 d . . . O10 O 0.4151(2) 0.25131(13) 0.07636(12) 0.0168(5) Uani 1 1 d . . . O11 O 0.3885(2) 0.26846(14) 0.19789(14) 0.0285(6) Uani 1 1 d . . . O12 O 0.3755(2) 0.29711(15) -0.14715(13) 0.0235(6) Uani 1 1 d . . . C1 C 0.4842(4) 0.1386(2) -0.0964(2) 0.0225(8) Uani 1 1 d . . . C2 C 0.7871(3) 0.0600(2) 0.0123(2) 0.0216(7) Uani 1 1 d . . . C3 C 0.3968(3) 0.0720(2) 0.1366(2) 0.0232(8) Uani 1 1 d . . . C4 C 0.7765(3) 0.1921(2) 0.1883(2) 0.0214(7) Uani 1 1 d . . . C5 C 0.6691(3) 0.32934(19) -0.0001(2) 0.0205(7) Uani 1 1 d . . . C6 C 0.3630(3) 0.2820(2) 0.1332(2) 0.0244(8) Uani 1 1 d . . . H1 H 0.876(5) 0.045(3) 0.015(3) 0.051(14) Uiso 1 1 d . . . H2 H 0.333(3) 0.034(2) 0.1322(18) 0.012(8) Uiso 1 1 d . . . H3 H 0.795(3) 0.1883(18) 0.2391(19) 0.011(8) Uiso 1 1 d . . . H4 H 0.741(3) 0.3665(18) -0.0053(17) 0.007(8) Uiso 1 1 d . . . H5 H 0.288(3) 0.322(2) 0.121(2) 0.023(10) Uiso 1 1 d . . . H6 H 0.469(3) 0.154(2) -0.142(2) 0.024(10) Uiso 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 Co1 0.0129(2) 0.0144(2) 0.0132(2) 0.00032(17) 0.00054(16) -0.00076(17) Co2 0.0130(2) 0.0163(2) 0.0155(2) 0.00152(18) -0.00125(16) 0.00095(17) Co3 0.0192(3) 0.0202(3) 0.0116(3) 0.000 0.0025(2) 0.000 Co4 0.0198(3) 0.0140(3) 0.0162(3) -0.0024(3) 0.0029(2) -0.0016(3) O1 0.0199(11) 0.0177(12) 0.0154(12) -0.0026(10) -0.0020(9) 0.0026(9) O2 0.0451(15) 0.0178(13) 0.0184(13) -0.0003(10) 0.0028(11) 0.0008(12) O3 0.0207(11) 0.0161(13) 0.0387(16) -0.0027(11) 0.0007(10) -0.0021(10) O4 0.0167(10) 0.0169(12) 0.0218(13) -0.0010(9) 0.0023(9) -0.0001(9) O5 0.0218(11) 0.0166(12) 0.0149(12) -0.0015(9) 0.0049(9) -0.0019(10) O6 0.0289(12) 0.0316(15) 0.0201(14) -0.0073(12) 0.0075(10) -0.0063(11) O7 0.0165(10) 0.0240(13) 0.0139(12) -0.0018(9) 0.0004(9) -0.0013(10) O8 0.0154(10) 0.0155(12) 0.0213(13) 0.0018(10) 0.0002(9) -0.0001(9) O9 0.0170(11) 0.0188(13) 0.0331(15) 0.0069(11) -0.0041(10) 0.0001(10) O10 0.0158(10) 0.0199(12) 0.0148(12) -0.0001(10) 0.0002(8) 0.0009(9) O11 0.0395(14) 0.0300(15) 0.0161(13) 0.0000(11) 0.0040(11) 0.0119(12) O12 0.0177(11) 0.0348(15) 0.0179(13) 0.0024(11) -0.0009(9) 0.0034(10) C1 0.0295(18) 0.0237(19) 0.0143(19) 0.0032(15) -0.0013(14) 0.0013(15) C2 0.0163(15) 0.0210(18) 0.028(2) -0.0036(15) -0.0015(14) 0.0033(14) C3 0.0255(17) 0.0189(18) 0.025(2) -0.0039(15) 0.0031(14) -0.0075(15) C4 0.0223(16) 0.028(2) 0.0135(18) 0.0043(14) 0.0005(13) -0.0014(14) C5 0.0186(15) 0.0164(17) 0.027(2) 0.0026(14) 0.0007(14) -0.0027(14) C6 0.0270(17) 0.026(2) 0.0197(19) 0.0009(15) 0.0032(14) 0.0038(16) _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 Co1 O5 2.051(2) . ? Co1 O7 2.085(2) . ? Co1 O1 2.094(2) . ? Co1 O8 2.101(2) . ? Co1 O10 2.103(2) . ? Co1 O4 2.110(2) . ? Co2 O12 2.045(2) . ? Co2 O9 2.050(2) . ? Co2 O1 2.086(2) . ? Co2 O8 2.108(2) 4_455 ? Co2 O4 2.110(2) 4_455 ? Co2 O10 2.116(2) . ? Co3 O11 2.071(3) 3_655 ? Co3 O11 2.071(3) . ? Co3 O6 2.078(3) . ? Co3 O6 2.078(3) 3_655 ? Co3 O7 2.119(2) . ? Co3 O7 2.119(2) 3_655 ? Co4 O3 2.062(2) 5_655 ? Co4 O3 2.062(2) . ? Co4 O2 2.093(2) . ? Co4 O2 2.093(2) 5_655 ? Co4 O5 2.129(2) 5_655 ? Co4 O5 2.129(2) . ? O1 C1 1.260(4) . ? O2 C1 1.233(4) . ? O3 C2 1.242(4) . ? O4 C2 1.273(4) . ? O4 Co2 2.110(2) 4 ? O5 C3 1.282(4) . ? O6 C3 1.224(4) . ? O7 C4 1.270(4) . ? O8 C5 1.266(4) . ? O8 Co2 2.108(2) 4 ? O9 C5 1.239(4) . ? O10 C6 1.278(4) . ? O11 C6 1.223(4) . ? O12 C4 1.245(4) 4_455 ? C4 O12 1.245(4) 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 O5 Co1 O7 94.20(9) . . ? O5 Co1 O1 90.36(9) . . ? O7 Co1 O1 172.74(9) . . ? O5 Co1 O8 173.60(9) . . ? O7 Co1 O8 88.80(9) . . ? O1 Co1 O8 87.24(9) . . ? O5 Co1 O10 96.95(9) . . ? O7 Co1 O10 96.28(9) . . ? O1 Co1 O10 77.54(9) . . ? O8 Co1 O10 88.33(9) . . ? O5 Co1 O4 95.52(9) . . ? O7 Co1 O4 92.41(9) . . ? O1 Co1 O4 92.77(9) . . ? O8 Co1 O4 78.68(9) . . ? O10 Co1 O4 164.22(9) . . ? O12 Co2 O9 93.45(10) . . ? O12 Co2 O1 92.76(10) . . ? O9 Co2 O1 94.58(9) . . ? O12 Co2 O8 91.81(9) . 4_455 ? O9 Co2 O8 170.23(10) . 4_455 ? O1 Co2 O8 93.39(9) . 4_455 ? O12 Co2 O4 88.76(9) . 4_455 ? O9 Co2 O4 93.33(9) . 4_455 ? O1 Co2 O4 171.84(9) . 4_455 ? O8 Co2 O4 78.55(9) 4_455 4_455 ? O12 Co2 O10 170.13(10) . . ? O9 Co2 O10 88.40(9) . . ? O1 Co2 O10 77.42(9) . . ? O8 Co2 O10 87.82(8) 4_455 . ? O4 Co2 O10 100.82(9) 4_455 . ? O11 Co3 O11 88.87(15) 3_655 . ? O11 Co3 O6 177.48(10) 3_655 . ? O11 Co3 O6 89.54(10) . . ? O11 Co3 O6 89.54(10) 3_655 3_655 ? O11 Co3 O6 177.48(10) . 3_655 ? O6 Co3 O6 92.12(15) . 3_655 ? O11 Co3 O7 86.67(9) 3_655 . ? O11 Co3 O7 94.04(9) . . ? O6 Co3 O7 91.51(9) . . ? O6 Co3 O7 87.81(9) 3_655 . ? O11 Co3 O7 94.04(9) 3_655 3_655 ? O11 Co3 O7 86.67(9) . 3_655 ? O6 Co3 O7 87.81(9) . 3_655 ? O6 Co3 O7 91.51(9) 3_655 3_655 ? O7 Co3 O7 179.01(13) . 3_655 ? O3 Co4 O3 180.00(13) 5_655 . ? O3 Co4 O2 89.07(10) 5_655 . ? O3 Co4 O2 90.93(10) . . ? O3 Co4 O2 90.93(10) 5_655 5_655 ? O3 Co4 O2 89.07(10) . 5_655 ? O2 Co4 O2 180.00(14) . 5_655 ? O3 Co4 O5 91.34(9) 5_655 5_655 ? O3 Co4 O5 88.66(9) . 5_655 ? O2 Co4 O5 85.11(9) . 5_655 ? O2 Co4 O5 94.89(9) 5_655 5_655 ? O3 Co4 O5 88.66(9) 5_655 . ? O3 Co4 O5 91.34(9) . . ? O2 Co4 O5 94.89(9) . . ? O2 Co4 O5 85.11(9) 5_655 . ? O5 Co4 O5 180.00(16) 5_655 . ? C1 O1 Co2 127.0(2) . . ? C1 O1 Co1 131.9(2) . . ? Co2 O1 Co1 99.58(10) . . ? C1 O2 Co4 133.5(2) . . ? C2 O3 Co4 133.1(2) . . ? C2 O4 Co2 127.4(2) . 4 ? C2 O4 Co1 133.0(2) . . ? Co2 O4 Co1 97.36(9) 4 . ? C3 O5 Co1 125.3(2) . . ? C3 O5 Co4 119.5(2) . . ? Co1 O5 Co4 115.19(10) . . ? C3 O6 Co3 139.4(2) . . ? C4 O7 Co1 127.7(2) . . ? C4 O7 Co3 119.1(2) . . ? Co1 O7 Co3 113.17(9) . . ? C5 O8 Co1 131.6(2) . . ? C5 O8 Co2 127.4(2) . 4 ? Co1 O8 Co2 97.68(9) . 4 ? C5 O9 Co2 127.7(2) . . ? C6 O10 Co1 133.7(2) . . ? C6 O10 Co2 126.4(2) . . ? Co1 O10 Co2 98.33(9) . . ? C6 O11 Co3 133.6(2) . . ? C4 O12 Co2 131.1(2) 4_455 . ? O2 C1 O1 126.0(4) . . ? O3 C2 O4 126.3(3) . . ? O6 C3 O5 127.2(3) . . ? O12 C4 O7 126.5(3) 4 . ? O9 C5 O8 126.7(3) . . ? O11 C6 O10 126.7(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.085 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.126 # Attachment '- CCDC_793420.cif' data_pbcn2 _database_code_depnum_ccdc_archive 'CCDC 793420' #TrackingRef '- CCDC_793420.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'magnesium(ii) formate DEF solvate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Mg6 O24' _chemical_formula_weight 686.08 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.8715(9) _cell_length_b 18.2678(15) _cell_length_c 18.1613(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3275.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3421 _cell_measurement_theta_min 2.345 _cell_measurement_theta_max 27.003 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9331 _exptl_absorpt_correction_T_max 0.9438 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'SMART CCD' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15380 _diffrn_reflns_av_R_equivalents 0.1385 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2890 _reflns_number_gt 2092 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material 'Diamond 3.1' _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 contributions of the disordered DEF molecules were removed from the diffraction data using the SQUEEZE routine of PLATON software (c.a. 229 e/u.c), and then final refinements were carried out. ; _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^)+(0.0574P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2890 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Mg1 Mg -0.07905(10) 0.31992(5) -0.06053(5) 0.0155(3) Uani 1 1 d . . . Mg2 Mg -0.38870(9) 0.28313(5) -0.03545(5) 0.0173(3) Uani 1 1 d . . . Mg3 Mg 0.0000 0.31223(8) -0.2500 0.0185(3) Uani 1 2 d S . . Mg4 Mg 0.0000 0.5000 0.0000 0.0187(3) Uani 1 2 d S . . O1 O -0.15281(19) 0.31303(11) -0.16782(10) 0.0186(5) Uani 1 1 d . . . O2 O -0.3735(2) 0.29469(12) -0.14608(11) 0.0245(5) Uani 1 1 d . . . O3 O -0.25585(19) 0.37100(11) -0.02240(11) 0.0190(5) Uani 1 1 d . . . O4 O -0.2063(2) 0.48969(11) -0.00802(12) 0.0273(5) Uani 1 1 d . . . O5 O -0.20014(19) 0.23023(11) -0.03133(11) 0.0175(5) Uani 1 1 d . . . O6 O -0.5575(2) 0.34611(11) -0.02608(12) 0.0231(5) Uani 1 1 d . . . O7 O 0.0030(2) 0.42815(12) 0.08680(11) 0.0270(5) Uani 1 1 d . . . O8 O 0.0054(2) 0.31346(10) 0.04506(11) 0.0181(5) Uani 1 1 d . . . O9 O 0.08166(19) 0.24740(11) -0.07548(10) 0.0173(5) Uani 1 1 d . . . O10 O 0.1074(2) 0.23245(12) -0.19687(11) 0.0284(6) Uani 1 1 d . . . O11 O 0.0261(2) 0.41571(11) -0.07917(10) 0.0192(5) Uani 1 1 d . . . O12 O 0.1037(2) 0.38970(12) -0.19186(11) 0.0259(5) Uani 1 1 d . . . C1 C -0.2763(3) 0.30614(18) -0.18731(18) 0.0245(8) Uani 1 1 d . . . C2 C -0.2865(3) 0.43809(17) -0.01253(17) 0.0225(7) Uani 1 1 d . . . C3 C -0.1691(3) 0.17038(18) -0.00021(18) 0.0221(7) Uani 1 1 d . . . C4 C 0.0169(3) 0.36161(19) 0.09512(17) 0.0241(8) Uani 1 1 d . . . C5 C 0.1338(3) 0.21842(19) -0.13216(18) 0.0269(8) Uani 1 1 d . . . C6 C 0.0999(3) 0.42702(19) -0.13569(17) 0.0240(7) Uani 1 1 d . . . H1 H -0.287(3) 0.3126(15) -0.2380(18) 0.022(9) Uiso 1 1 d . . . H2 H -0.384(4) 0.4496(17) -0.0063(18) 0.032(9) Uiso 1 1 d . . . H3 H -0.233(3) 0.1352(17) 0.0049(15) 0.017(8) Uiso 1 1 d . . . H4 H 0.036(2) 0.3463(14) 0.1444(15) 0.004(6) Uiso 1 1 d . . . H5 H 0.208(4) 0.1779(18) -0.1201(18) 0.037(10) Uiso 1 1 d . . . H6 H 0.158(3) 0.471(2) -0.1317(18) 0.034(9) Uiso 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 Mg1 0.0124(5) 0.0194(6) 0.0148(5) 0.0004(4) 0.0001(4) 0.0002(4) Mg2 0.0118(5) 0.0219(6) 0.0181(5) 0.0017(4) 0.0016(4) -0.0016(4) Mg3 0.0173(8) 0.0244(9) 0.0139(7) 0.000 0.0025(6) 0.000 Mg4 0.0170(7) 0.0199(8) 0.0193(7) -0.0012(6) 0.0017(6) -0.0015(6) O1 0.0132(11) 0.0290(13) 0.0136(10) 0.0008(9) 0.0001(8) -0.0016(9) O2 0.0156(11) 0.0388(14) 0.0192(11) 0.0021(10) 0.0018(9) -0.0045(10) O3 0.0155(11) 0.0197(12) 0.0218(11) -0.0014(9) 0.0023(9) 0.0004(9) O4 0.0211(12) 0.0205(12) 0.0404(14) -0.0063(10) 0.0009(10) -0.0023(10) O5 0.0129(11) 0.0183(11) 0.0213(11) 0.0029(9) 0.0024(9) 0.0015(8) O6 0.0139(11) 0.0236(12) 0.0317(12) 0.0044(10) 0.0046(9) -0.0001(9) O7 0.0411(15) 0.0170(13) 0.0230(12) -0.0034(10) 0.0009(10) -0.0004(10) O8 0.0168(11) 0.0232(12) 0.0142(10) 0.0000(9) -0.0012(8) 0.0011(9) O9 0.0147(11) 0.0211(12) 0.0161(10) -0.0010(9) 0.0022(9) 0.0041(9) O10 0.0349(14) 0.0335(14) 0.0168(12) 0.0007(10) 0.0031(10) 0.0111(10) O11 0.0189(11) 0.0199(12) 0.0189(11) -0.0009(9) 0.0042(9) -0.0044(9) O12 0.0236(13) 0.0343(14) 0.0197(12) -0.0067(11) 0.0054(9) -0.0051(10) C1 0.0276(19) 0.032(2) 0.0135(17) 0.0024(15) -0.0005(14) -0.0019(15) C2 0.0163(17) 0.026(2) 0.0252(18) -0.0027(15) 0.0010(13) 0.0063(15) C3 0.0152(17) 0.0235(18) 0.0277(17) 0.0004(15) 0.0016(14) -0.0059(15) C4 0.0276(18) 0.034(2) 0.0103(16) 0.0022(15) 0.0008(14) -0.0019(16) C5 0.028(2) 0.028(2) 0.0246(19) 0.0018(16) 0.0043(15) 0.0084(15) C6 0.0260(19) 0.0246(19) 0.0215(17) 0.0006(16) 0.0061(14) -0.0037(15) _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 Mg1 O11 2.063(2) . ? Mg1 O1 2.084(2) . ? Mg1 O9 2.085(2) . ? Mg1 O8 2.094(2) . ? Mg1 O5 2.096(2) . ? Mg1 O3 2.097(2) . ? Mg1 Mg2 3.1628(14) . ? Mg1 Mg2 3.1800(13) 4 ? Mg1 Mg3 3.5311(10) . ? Mg1 Mg4 3.5553(10) . ? Mg2 O2 2.026(2) . ? Mg2 O6 2.032(2) . ? Mg2 O8 2.058(2) 4_455 ? Mg2 O3 2.086(2) . ? Mg2 O5 2.099(2) . ? Mg2 O9 2.111(2) 4_455 ? Mg2 Mg1 3.1800(13) 4_455 ? Mg3 O12 2.041(2) . ? Mg3 O12 2.041(2) 3_554 ? Mg3 O10 2.044(2) 3_554 ? Mg3 O10 2.044(2) . ? Mg3 O1 2.1221(19) . ? Mg3 O1 2.1221(19) 3_554 ? Mg3 Mg1 3.5311(10) 3_554 ? Mg4 O4 2.050(2) . ? Mg4 O4 2.050(2) 5_565 ? Mg4 O7 2.052(2) . ? Mg4 O7 2.052(2) 5_565 ? Mg4 O11 2.122(2) . ? Mg4 O11 2.122(2) 5_565 ? Mg4 Mg1 3.5553(10) 5_565 ? O1 C1 1.275(4) . ? O2 C1 1.235(4) . ? O3 C2 1.275(4) . ? O4 C2 1.233(4) . ? O5 C3 1.268(4) . ? O6 C3 1.238(4) 4_455 ? O7 C4 1.232(4) . ? O8 C4 1.270(4) . ? O8 Mg2 2.058(2) 4 ? O9 C5 1.267(4) . ? O9 Mg2 2.111(2) 4 ? O10 C5 1.231(4) . ? O11 C6 1.275(4) . ? O12 C6 1.228(4) . ? C3 O6 1.238(4) 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 O11 Mg1 O1 94.23(8) . . ? O11 Mg1 O9 97.74(9) . . ? O1 Mg1 O9 96.07(8) . . ? O11 Mg1 O8 89.87(9) . . ? O1 Mg1 O8 172.67(9) . . ? O9 Mg1 O8 77.33(8) . . ? O11 Mg1 O5 172.56(9) . . ? O1 Mg1 O5 89.43(8) . . ? O9 Mg1 O5 88.29(8) . . ? O8 Mg1 O5 87.20(8) . . ? O11 Mg1 O3 95.49(8) . . ? O1 Mg1 O3 92.57(8) . . ? O9 Mg1 O3 163.60(9) . . ? O8 Mg1 O3 93.09(9) . . ? O5 Mg1 O3 77.86(8) . . ? O11 Mg1 Mg2 133.66(7) . . ? O1 Mg1 Mg2 77.54(6) . . ? O9 Mg1 Mg2 128.26(7) . . ? O8 Mg1 Mg2 103.93(7) . . ? O5 Mg1 Mg2 41.09(6) . . ? O3 Mg1 Mg2 40.76(6) . . ? O11 Mg1 Mg2 107.14(7) . 4 ? O1 Mg1 Mg2 133.10(7) . 4 ? O9 Mg1 Mg2 41.02(6) . 4 ? O8 Mg1 Mg2 39.61(6) . 4 ? O5 Mg1 Mg2 74.67(6) . 4 ? O3 Mg1 Mg2 125.04(7) . 4 ? Mg2 Mg1 Mg2 111.49(3) . 4 ? O11 Mg1 Mg3 76.27(6) . . ? O1 Mg1 Mg3 33.25(5) . . ? O9 Mg1 Mg3 71.32(6) . . ? O8 Mg1 Mg3 143.33(7) . . ? O5 Mg1 Mg3 109.97(7) . . ? O3 Mg1 Mg3 121.57(7) . . ? Mg2 Mg1 Mg3 110.21(3) . . ? Mg2 Mg1 Mg3 112.34(3) 4 . ? O11 Mg1 Mg4 32.36(6) . . ? O1 Mg1 Mg4 114.94(7) . . ? O9 Mg1 Mg4 117.47(6) . . ? O8 Mg1 Mg4 71.43(6) . . ? O5 Mg1 Mg4 140.36(6) . . ? O3 Mg1 Mg4 70.66(6) . . ? Mg2 Mg1 Mg4 111.36(3) . . ? Mg2 Mg1 Mg4 104.39(3) 4 . ? Mg3 Mg1 Mg4 106.83(3) . . ? O2 Mg2 O6 94.87(9) . . ? O2 Mg2 O8 92.46(9) . 4_455 ? O6 Mg2 O8 94.36(9) . 4_455 ? O2 Mg2 O3 89.18(9) . . ? O6 Mg2 O3 94.03(9) . . ? O8 Mg2 O3 171.29(9) 4_455 . ? O2 Mg2 O5 91.00(9) . . ? O6 Mg2 O5 170.07(10) . . ? O8 Mg2 O5 93.38(9) 4_455 . ? O3 Mg2 O5 78.03(8) . . ? O2 Mg2 O9 169.88(10) . 4_455 ? O6 Mg2 O9 87.48(9) . 4_455 ? O8 Mg2 O9 77.53(8) 4_455 4_455 ? O3 Mg2 O9 100.49(8) . 4_455 ? O5 Mg2 O9 88.13(8) . 4_455 ? O2 Mg2 Mg1 76.30(6) . . ? O6 Mg2 Mg1 133.17(7) . . ? O8 Mg2 Mg1 131.37(7) 4_455 . ? O3 Mg2 Mg1 41.00(6) . . ? O5 Mg2 Mg1 41.04(6) . . ? O9 Mg2 Mg1 109.12(6) 4_455 . ? O2 Mg2 Mg1 130.48(7) . 4_455 ? O6 Mg2 Mg1 78.74(6) . 4_455 ? O8 Mg2 Mg1 40.44(6) 4_455 4_455 ? O3 Mg2 Mg1 139.87(7) . 4_455 ? O5 Mg2 Mg1 103.42(7) . 4_455 ? O9 Mg2 Mg1 40.41(6) 4_455 4_455 ? Mg1 Mg2 Mg1 140.88(4) . 4_455 ? O12 Mg3 O12 92.21(13) . 3_554 ? O12 Mg3 O10 177.01(8) . 3_554 ? O12 Mg3 O10 89.43(9) 3_554 3_554 ? O12 Mg3 O10 89.43(9) . . ? O12 Mg3 O10 177.01(8) 3_554 . ? O10 Mg3 O10 89.05(13) 3_554 . ? O12 Mg3 O1 89.31(8) . . ? O12 Mg3 O1 90.15(8) 3_554 . ? O10 Mg3 O1 88.18(8) 3_554 . ? O10 Mg3 O1 92.38(8) . . ? O12 Mg3 O1 90.15(8) . 3_554 ? O12 Mg3 O1 89.31(8) 3_554 3_554 ? O10 Mg3 O1 92.38(8) 3_554 3_554 ? O10 Mg3 O1 88.18(8) . 3_554 ? O1 Mg3 O1 179.22(13) . 3_554 ? O12 Mg3 Mg1 65.11(6) . . ? O12 Mg3 Mg1 111.45(6) 3_554 . ? O10 Mg3 Mg1 111.94(6) 3_554 . ? O10 Mg3 Mg1 71.52(6) . . ? O1 Mg3 Mg1 32.57(5) . . ? O1 Mg3 Mg1 147.37(5) 3_554 . ? O12 Mg3 Mg1 111.45(6) . 3_554 ? O12 Mg3 Mg1 65.11(6) 3_554 3_554 ? O10 Mg3 Mg1 71.52(6) 3_554 3_554 ? O10 Mg3 Mg1 111.94(6) . 3_554 ? O1 Mg3 Mg1 147.37(5) . 3_554 ? O1 Mg3 Mg1 32.57(5) 3_554 3_554 ? Mg1 Mg3 Mg1 175.45(5) . 3_554 ? O4 Mg4 O4 180.00(13) . 5_565 ? O4 Mg4 O7 90.58(9) . . ? O4 Mg4 O7 89.42(9) 5_565 . ? O4 Mg4 O7 89.42(9) . 5_565 ? O4 Mg4 O7 90.58(9) 5_565 5_565 ? O7 Mg4 O7 180.00(12) . 5_565 ? O4 Mg4 O11 90.34(8) . . ? O4 Mg4 O11 89.66(8) 5_565 . ? O7 Mg4 O11 93.13(8) . . ? O7 Mg4 O11 86.87(8) 5_565 . ? O4 Mg4 O11 89.66(8) . 5_565 ? O4 Mg4 O11 90.34(8) 5_565 5_565 ? O7 Mg4 O11 86.87(8) . 5_565 ? O7 Mg4 O11 93.13(8) 5_565 5_565 ? O11 Mg4 O11 180.00(11) . 5_565 ? O4 Mg4 Mg1 71.04(6) . . ? O4 Mg4 Mg1 108.96(6) 5_565 . ? O7 Mg4 Mg1 69.44(6) . . ? O7 Mg4 Mg1 110.56(6) 5_565 . ? O11 Mg4 Mg1 31.34(5) . . ? O11 Mg4 Mg1 148.66(5) 5_565 . ? O4 Mg4 Mg1 108.96(6) . 5_565 ? O4 Mg4 Mg1 71.04(6) 5_565 5_565 ? O7 Mg4 Mg1 110.56(6) . 5_565 ? O7 Mg4 Mg1 69.44(6) 5_565 5_565 ? O11 Mg4 Mg1 148.66(5) . 5_565 ? O11 Mg4 Mg1 31.34(5) 5_565 5_565 ? Mg1 Mg4 Mg1 180.00(3) . 5_565 ? C1 O1 Mg1 126.83(19) . . ? C1 O1 Mg3 118.90(19) . . ? Mg1 O1 Mg3 114.18(9) . . ? C1 O2 Mg2 132.6(2) . . ? C2 O3 Mg2 127.33(19) . . ? C2 O3 Mg1 132.19(19) . . ? Mg2 O3 Mg1 98.24(9) . . ? C2 O4 Mg4 135.4(2) . . ? C3 O5 Mg1 130.45(19) . . ? C3 O5 Mg2 128.83(19) . . ? Mg1 O5 Mg2 97.87(9) . . ? C3 O6 Mg2 128.6(2) 4_455 . ? C4 O7 Mg4 136.6(2) . . ? C4 O8 Mg2 127.5(2) . 4 ? C4 O8 Mg1 130.7(2) . . ? Mg2 O8 Mg1 99.95(9) 4 . ? C5 O9 Mg1 132.9(2) . . ? C5 O9 Mg2 127.5(2) . 4 ? Mg1 O9 Mg2 98.57(9) . 4 ? C5 O10 Mg3 135.1(2) . . ? C6 O11 Mg1 123.8(2) . . ? C6 O11 Mg4 119.8(2) . . ? Mg1 O11 Mg4 116.30(9) . . ? C6 O12 Mg3 143.1(2) . . ? O2 C1 O1 126.2(3) . . ? O4 C2 O3 126.3(3) . . ? O6 C3 O5 126.6(3) 4 . ? O7 C4 O8 125.8(3) . . ? O10 C5 O9 127.1(3) . . ? O12 C6 O11 126.6(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.432 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.074 # Attachment '- CCDC_793421.cif' data_pbcn3 _database_code_depnum_ccdc_archive 'CCDC 793421' #TrackingRef '- CCDC_793421.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Zinc(ii) formate DEF solvate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 O24 Zn6' _chemical_formula_weight 932.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.8680(4) _cell_length_b 18.2476(8) _cell_length_c 18.1400(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3266.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12403 _cell_measurement_theta_min 2.346 _cell_measurement_theta_max 28.282 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 4.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2845 _exptl_absorpt_correction_T_max 0.4719 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'SMART CCD' _diffrn_measurement_method Omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18069 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3990 _reflns_number_gt 3543 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material 'Diamond 3.1' _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 contributions of the disordered DEF molecules were removed from the diffraction data using the SQUEEZE routine of PLATON software (c.a. 164 e/u.c), and then final refinements were carried out. ; _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^)+(0.0582P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3990 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _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 0.07747(3) 0.321295(13) 0.062216(13) 0.01635(9) Uani 1 1 d . . . Zn2 Zn -0.10991(3) 0.215225(13) -0.035846(14) 0.01821(9) Uani 1 1 d . . . Zn3 Zn 0.0000 0.31118(2) 0.2500 0.02091(10) Uani 1 2 d S . . Zn4 Zn 0.0000 0.5000 0.0000 0.02004(10) Uani 1 2 d S . . O1 O -0.02649(17) 0.41587(8) 0.08097(8) 0.0208(3) Uani 1 1 d . . . O2 O -0.10819(19) 0.39092(10) 0.19320(9) 0.0300(4) Uani 1 1 d . . . O3 O -0.08387(16) 0.24764(9) 0.07702(9) 0.0203(3) Uani 1 1 d . . . O4 O -0.1102(2) 0.23017(10) 0.19796(9) 0.0322(4) Uani 1 1 d . . . O5 O -0.00741(17) 0.31468(8) -0.04476(9) 0.0198(3) Uani 1 1 d . . . O6 O -0.0022(2) 0.42837(9) -0.08994(10) 0.0319(4) Uani 1 1 d . . . O7 O 0.19828(16) 0.23025(8) 0.03144(8) 0.0197(3) Uani 1 1 d . . . O8 O 0.05919(18) 0.15222(9) -0.02663(10) 0.0266(4) Uani 1 1 d . . . O9 O 0.15457(17) 0.31316(9) 0.16831(8) 0.0211(3) Uani 1 1 d . . . O10 O 0.20881(19) 0.49237(9) 0.00873(10) 0.0292(4) Uani 1 1 d . . . O11 O -0.12298(17) 0.20408(10) -0.14752(9) 0.0262(4) Uani 1 1 d . . . O12 O -0.24513(16) 0.12732(8) -0.02123(9) 0.0204(3) Uani 1 1 d . . . C1 C -0.1011(3) 0.42809(13) 0.13714(13) 0.0248(5) Uani 1 1 d . . . C2 C -0.1360(3) 0.21677(13) 0.13286(14) 0.0262(5) Uani 1 1 d . . . C3 C -0.0172(3) 0.36148(13) -0.09610(13) 0.0247(5) Uani 1 1 d . . . C4 C 0.1704(2) 0.17018(12) -0.00047(13) 0.0220(5) Uani 1 1 d . . . C5 C 0.2778(3) 0.30618(13) 0.18821(12) 0.0252(5) Uani 1 1 d . . . C6 C 0.2876(3) 0.43968(13) 0.01266(14) 0.0247(5) Uani 1 1 d . . . H1 H -0.151(3) 0.4662(18) 0.1334(17) 0.031(7) Uiso 1 1 d . . . H2 H -0.200(3) 0.1796(16) 0.1224(18) 0.036(8) Uiso 1 1 d . . . H3 H 0.240(3) 0.1371(16) -0.0061(15) 0.026(7) Uiso 1 1 d . . . H4 H -0.038(3) 0.3440(17) -0.1424(17) 0.027(7) Uiso 1 1 d . . . H5 H 0.302(3) 0.3117(13) 0.2391(16) 0.025(7) Uiso 1 1 d . . . H6 H 0.381(3) 0.4489(14) 0.0128(15) 0.020(6) Uiso 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 0.01702(14) 0.01638(14) 0.01566(14) -0.00068(8) 0.00028(9) 0.00059(9) Zn2 0.01702(15) 0.01864(14) 0.01898(15) -0.00196(9) -0.00170(9) -0.00126(9) Zn3 0.0245(2) 0.0234(2) 0.01480(18) 0.000 0.00355(13) 0.000 Zn4 0.0247(2) 0.01612(18) 0.01929(19) 0.00304(12) 0.00276(13) 0.00132(14) O1 0.0252(8) 0.0178(7) 0.0194(7) 0.0025(6) 0.0051(6) 0.0044(6) O2 0.0351(10) 0.0313(9) 0.0235(8) 0.0091(7) 0.0095(7) 0.0085(7) O3 0.0209(8) 0.0234(8) 0.0166(7) 0.0007(6) 0.0007(6) -0.0023(6) O4 0.0447(11) 0.0327(9) 0.0192(8) 0.0000(7) 0.0038(7) -0.0140(8) O5 0.0221(8) 0.0190(8) 0.0182(7) 0.0015(6) -0.0035(6) -0.0020(6) O6 0.0546(13) 0.0182(8) 0.0230(8) 0.0023(6) 0.0003(8) 0.0010(8) O7 0.0174(8) 0.0176(7) 0.0240(8) -0.0015(6) 0.0005(6) 0.0007(6) O8 0.0223(8) 0.0215(8) 0.0360(9) -0.0071(7) -0.0063(8) 0.0003(7) O9 0.0213(8) 0.0266(8) 0.0154(7) -0.0023(6) 0.0006(6) 0.0017(6) O10 0.0256(9) 0.0177(8) 0.0444(10) 0.0049(7) 0.0000(8) 0.0004(7) O11 0.0214(8) 0.0368(9) 0.0205(8) -0.0034(7) -0.0009(7) -0.0035(7) O12 0.0208(8) 0.0159(7) 0.0244(7) 0.0017(6) -0.0023(6) -0.0007(6) C1 0.0294(12) 0.0195(10) 0.0254(11) 0.0029(9) 0.0059(9) 0.0069(10) C2 0.0295(12) 0.0262(11) 0.0228(11) -0.0019(9) 0.0033(10) -0.0102(10) C3 0.0333(13) 0.0244(11) 0.0164(10) 0.0002(8) -0.0006(9) -0.0004(10) C4 0.0202(11) 0.0190(10) 0.0268(11) -0.0034(8) -0.0002(9) 0.0043(9) C5 0.0274(12) 0.0318(12) 0.0163(10) -0.0031(9) -0.0008(9) 0.0026(10) C6 0.0192(11) 0.0225(11) 0.0322(11) 0.0035(9) 0.0004(10) -0.0030(9) _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 2.0363(15) . ? Zn1 O9 2.0748(16) . ? Zn1 O3 2.1009(16) . ? Zn1 O5 2.1170(16) . ? Zn1 O7 2.1197(15) . ? Zn1 O12 2.1205(16) 4 ? Zn2 O8 2.0332(17) . ? Zn2 O11 2.0401(17) . ? Zn2 O5 2.0839(15) . ? Zn2 O12 2.1033(15) . ? Zn2 O7 2.1399(16) 4_455 ? Zn2 O3 2.1465(16) . ? Zn3 O4 2.0639(18) . ? Zn3 O4 2.0639(18) 3 ? Zn3 O2 2.0782(17) 3 ? Zn3 O2 2.0782(17) . ? Zn3 O9 2.1269(16) . ? Zn3 O9 2.1269(16) 3 ? Zn4 O10 2.0713(19) 5_565 ? Zn4 O10 2.0713(19) . ? Zn4 O6 2.0907(18) . ? Zn4 O6 2.0907(18) 5_565 ? Zn4 O1 2.1407(15) 5_565 ? Zn4 O1 2.1407(15) . ? O1 C1 1.277(3) . ? O2 C1 1.224(3) . ? O3 C2 1.268(3) . ? O4 C2 1.232(3) . ? O5 C3 1.267(3) . ? O6 C3 1.235(3) . ? O7 C4 1.270(3) . ? O7 Zn2 2.1399(16) 4 ? O8 C4 1.240(3) . ? O9 C5 1.275(3) . ? O10 C6 1.238(3) . ? O11 C5 1.240(3) 4_455 ? O12 C6 1.274(3) 4_455 ? O12 Zn1 2.1205(16) 4_455 ? C5 O11 1.240(3) 4 ? C6 O12 1.274(3) 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 O9 95.19(6) . . ? O1 Zn1 O3 97.99(6) . . ? O9 Zn1 O3 96.52(6) . . ? O1 Zn1 O5 90.12(6) . . ? O9 Zn1 O5 172.42(6) . . ? O3 Zn1 O5 77.34(6) . . ? O1 Zn1 O7 172.58(6) . . ? O9 Zn1 O7 88.97(6) . . ? O3 Zn1 O7 87.62(6) . . ? O5 Zn1 O7 86.35(6) . . ? O1 Zn1 O12 95.72(6) . 4 ? O9 Zn1 O12 93.10(6) . 4 ? O3 Zn1 O12 162.43(6) . 4 ? O5 Zn1 O12 91.75(6) . 4 ? O7 Zn1 O12 77.87(6) . 4 ? O8 Zn2 O11 94.43(7) . . ? O8 Zn2 O5 95.77(7) . . ? O11 Zn2 O5 92.32(7) . . ? O8 Zn2 O12 94.54(7) . . ? O11 Zn2 O12 90.51(6) . . ? O5 Zn2 O12 169.07(6) . . ? O8 Zn2 O7 170.32(7) . 4_455 ? O11 Zn2 O7 91.58(6) . 4_455 ? O5 Zn2 O7 91.56(6) . 4_455 ? O12 Zn2 O7 77.80(6) . 4_455 ? O8 Zn2 O3 88.80(7) . . ? O11 Zn2 O3 169.17(7) . . ? O5 Zn2 O3 77.05(6) . . ? O12 Zn2 O3 99.55(6) . . ? O7 Zn2 O3 86.68(6) 4_455 . ? O4 Zn3 O4 88.51(11) . 3 ? O4 Zn3 O2 177.50(7) . 3 ? O4 Zn3 O2 90.23(8) 3 3 ? O4 Zn3 O2 90.23(8) . . ? O4 Zn3 O2 177.50(7) 3 . ? O2 Zn3 O2 91.11(11) 3 . ? O4 Zn3 O9 94.10(7) . . ? O4 Zn3 O9 87.30(7) 3 . ? O2 Zn3 O9 88.00(6) 3 . ? O2 Zn3 O9 90.63(6) . . ? O4 Zn3 O9 87.30(7) . 3 ? O4 Zn3 O9 94.10(7) 3 3 ? O2 Zn3 O9 90.63(6) 3 3 ? O2 Zn3 O9 88.00(6) . 3 ? O9 Zn3 O9 178.05(9) . 3 ? O10 Zn4 O10 180.00(10) 5_565 . ? O10 Zn4 O6 88.39(7) 5_565 . ? O10 Zn4 O6 91.61(7) . . ? O10 Zn4 O6 91.61(7) 5_565 5_565 ? O10 Zn4 O6 88.39(7) . 5_565 ? O6 Zn4 O6 180.00(10) . 5_565 ? O10 Zn4 O1 91.19(7) 5_565 5_565 ? O10 Zn4 O1 88.81(7) . 5_565 ? O6 Zn4 O1 85.07(6) . 5_565 ? O6 Zn4 O1 94.93(6) 5_565 5_565 ? O10 Zn4 O1 88.81(7) 5_565 . ? O10 Zn4 O1 91.19(7) . . ? O6 Zn4 O1 94.93(6) . . ? O6 Zn4 O1 85.07(6) 5_565 . ? O1 Zn4 O1 180.00(8) 5_565 . ? C1 O1 Zn1 124.89(15) . . ? C1 O1 Zn4 119.52(14) . . ? Zn1 O1 Zn4 115.57(7) . . ? C1 O2 Zn3 140.37(17) . . ? C2 O3 Zn1 133.92(15) . . ? C2 O3 Zn2 126.23(15) . . ? Zn1 O3 Zn2 98.34(6) . . ? C2 O4 Zn3 133.55(16) . . ? C3 O5 Zn2 127.35(15) . . ? C3 O5 Zn1 131.72(15) . . ? Zn2 O5 Zn1 99.82(6) . . ? C3 O6 Zn4 133.63(16) . . ? C4 O7 Zn1 132.45(15) . . ? C4 O7 Zn2 127.59(15) . 4 ? Zn1 O7 Zn2 97.08(6) . 4 ? C4 O8 Zn2 127.49(15) . . ? C5 O9 Zn1 128.28(15) . . ? C5 O9 Zn3 119.02(14) . . ? Zn1 O9 Zn3 112.61(8) . . ? C6 O10 Zn4 132.91(16) . . ? C5 O11 Zn2 130.98(16) 4_455 . ? C6 O12 Zn2 125.91(15) 4_455 . ? C6 O12 Zn1 132.56(15) 4_455 4_455 ? Zn2 O12 Zn1 98.18(6) . 4_455 ? O2 C1 O1 126.8(2) . . ? O4 C2 O3 126.4(2) . . ? O6 C3 O5 126.2(2) . . ? O8 C4 O7 126.5(2) . . ? O11 C5 O9 126.8(2) 4 . ? O10 C6 O12 126.4(2) . 4 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.902 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.121