# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'L. Brammer' _publ_contact_author_address ; Department of Chemistry University of Sheffield Brook Hill Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_email LEE.BRAMMER@SHEFFIELD.AC.UK _publ_section_title ; Ligand Flexibility and Framework Rearrangement in a New Family of Porous Metal-Organic Frameworks ; loop_ _publ_author_name 'L. Brammer' 'Darren Bradshaw' 'Guillermo Minguez Espallargas' 'Alastair Florence' 'Samuel M. Hawxwell' ; T.J.Prior ; 'M J. Rosseinsky' 'J.van de Streek' data_dl102m _database_code_depnum_ccdc_archive 'CCDC 632264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 O14 Zn2, H2 O, H2 O' _chemical_formula_sum 'C20 H26 O16 Zn2' _chemical_formula_weight 326.57 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6916(15) _cell_length_b 8.5113(17) _cell_length_c 9.827(2) _cell_angle_alpha 68.56(3) _cell_angle_beta 79.47(3) _cell_angle_gamma 86.62(3) _cell_volume 588.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1727 _cell_measurement_theta_min 7.623 _cell_measurement_theta_max 64.361 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 334 _exptl_absorpt_coefficient_mu 2.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8833 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.84600 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'SRS station 16.2smx' _diffrn_radiation_monochromator silicon(111) _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'fine slice \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4270 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 32.87 _reflns_number_total 2358 _reflns_number_gt 2152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0632P)^2^+1.1991P] 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 2358 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.47070(5) 0.34872(5) 1.38422(4) 0.00737(17) Uani 1 1 d . . . O1 O 0.2979(4) 0.1145(3) 1.3653(3) 0.0144(6) Uani 1 1 d . . . O2 O 0.4360(4) 0.3392(3) 1.1914(3) 0.0111(6) Uani 1 1 d . . . O3 O 0.1651(3) -0.2399(3) 1.0868(3) 0.0081(5) Uani 1 1 d . . . O4 O 0.3785(4) 0.2384(3) 0.5984(3) 0.0117(6) Uani 1 1 d . . . O5 O 0.3559(3) 0.4659(3) 0.6614(3) 0.0091(5) Uani 1 1 d . . . C1 C 0.3535(5) 0.2003(5) 1.2305(4) 0.0088(7) Uani 1 1 d . . . C2 C 0.3552(5) 0.3090(5) 0.6922(4) 0.0077(7) Uani 1 1 d . . . C3 C 0.3188(5) 0.1420(4) 1.1118(4) 0.0061(7) Uani 1 1 d . . . C4 C 0.3524(4) 0.2511(4) 0.9626(4) 0.0057(7) Uani 1 1 d . . . H4 H 0.3966 0.3621 0.9365 0.007 Uiso 1 1 calc R . . C5 C 0.3198(5) 0.1938(4) 0.8533(4) 0.0063(7) Uani 1 1 d . . . C6 C 0.2595(5) 0.0294(4) 0.8900(4) 0.0063(7) Uani 1 1 d . . . H6 H 0.2417 -0.0098 0.8146 0.008 Uiso 1 1 calc R . . C7 C 0.2259(5) -0.0769(4) 1.0392(4) 0.0061(7) Uani 1 1 d . . . C8 C 0.2536(5) -0.0191(4) 1.1495(4) 0.0075(7) Uani 1 1 d . . . H8 H 0.2276 -0.0909 1.2509 0.009 Uiso 1 1 calc R . . C9 C 0.1183(5) -0.2973(4) 0.9766(4) 0.0080(7) Uani 1 1 d . . . H9A H 0.2255 -0.3040 0.9059 0.010 Uiso 1 1 calc R . . H9B H 0.0354 -0.2171 0.9203 0.010 Uiso 1 1 calc R . . C10 C 0.0321(5) -0.4698(4) 1.0557(4) 0.0062(7) Uani 1 1 d . . . H10A H -0.0692 -0.4641 1.1320 0.007 Uiso 1 1 calc R . . H10B H 0.1183 -0.5512 1.1063 0.007 Uiso 1 1 calc R . . O1W O 0.2438(4) 0.5313(3) 1.3582(3) 0.0124(6) Uani 1 1 d . . . H1WA H 0.2285 0.6096 1.4092 0.015 Uiso 1 1 d R . . H1WB H 0.1863 0.5990 1.2774 0.015 Uiso 1 1 d R . . O2W O 0.6854(4) 0.1824(3) 1.3997(3) 0.0129(6) Uani 1 1 d . . . H2WA H 0.8097 0.2079 1.3764 0.016 Uiso 1 1 d R . . H2WB H 0.6883 0.0849 1.4881 0.016 Uiso 1 1 d R . . O3W O 0.9794(4) 0.2764(4) 1.4749(3) 0.0213(7) Uani 1 1 d . . . H3WA H 1.0470 0.3787 1.4432 0.026 Uiso 1 1 d R . . H3WB H 1.0548 0.1825 1.4747 0.026 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0139(3) 0.0060(3) 0.0011(2) 0.00056(17) -0.00091(16) -0.00486(17) O1 0.0272(16) 0.0120(14) 0.0034(12) -0.0010(11) -0.0052(11) 0.0015(12) O2 0.0203(14) 0.0068(13) 0.0097(13) -0.0041(11) -0.0079(11) -0.0033(11) O3 0.0176(14) 0.0038(12) 0.0022(11) 0.0010(10) -0.0031(10) -0.0047(10) O4 0.0242(15) 0.0087(13) 0.0008(12) -0.0010(10) 0.0009(10) -0.0036(11) O5 0.0128(13) 0.0053(12) 0.0076(12) -0.0005(10) -0.0003(10) -0.0036(10) C1 0.0112(18) 0.0116(18) 0.0073(17) -0.0060(15) -0.0064(14) 0.0034(14) C2 0.0100(17) 0.0070(17) 0.0050(17) -0.0001(14) -0.0023(13) -0.0016(14) C3 0.0089(17) 0.0057(17) 0.0060(17) -0.0041(14) -0.0029(13) 0.0020(13) C4 0.0066(16) 0.0048(16) 0.0040(16) 0.0006(13) -0.0015(13) -0.0010(13) C5 0.0067(16) 0.0066(17) 0.0042(16) -0.0013(14) 0.0004(13) 0.0013(13) C6 0.0087(17) 0.0047(17) 0.0061(17) -0.0023(14) -0.0016(13) -0.0015(14) C7 0.0066(16) 0.0031(16) 0.0089(17) -0.0019(14) -0.0025(13) -0.0011(13) C8 0.0121(17) 0.0059(17) 0.0031(16) -0.0001(14) -0.0021(13) 0.0023(14) C9 0.0138(18) 0.0061(17) 0.0033(16) -0.0007(14) -0.0004(13) -0.0035(14) C10 0.0094(17) 0.0026(16) 0.0057(16) -0.0001(14) -0.0017(13) -0.0007(13) O1W 0.0184(14) 0.0104(13) 0.0084(13) -0.0029(11) -0.0042(11) 0.0027(11) O2W 0.0151(14) 0.0098(13) 0.0107(13) 0.0000(11) -0.0021(11) -0.0003(11) O3W 0.0172(15) 0.0226(16) 0.0213(16) -0.0053(13) -0.0003(12) -0.0060(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.976(3) 1_556 ? Zn1 O2 1.992(3) . ? Zn1 O5 1.995(3) 2_667 ? Zn1 O2W 2.101(3) . ? Zn1 O1W 2.254(3) . ? Zn1 C1 2.592(4) . ? O1 C1 1.262(5) . ? O2 C1 1.271(5) . ? O3 C7 1.373(4) . ? O3 C9 1.447(4) . ? O4 C2 1.255(5) . ? O4 Zn1 1.976(3) 1_554 ? O5 C2 1.257(4) . ? O5 Zn1 1.995(3) 2_667 ? C1 C3 1.494(5) . ? C2 C5 1.511(5) . ? C3 C8 1.383(5) . ? C3 C4 1.404(5) . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.396(5) . ? C6 C7 1.398(5) . ? C6 H6 0.9500 . ? C7 C8 1.395(5) . ? C8 H8 0.9500 . ? C9 C10 1.514(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C10 1.532(7) 2_547 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O1W H1WA 0.9600 . ? O1W H1WB 0.9600 . ? O2W H2WA 0.9600 . ? O2W H2WB 0.9600 . ? O3W H3WA 0.9600 . ? O3W H3WB 0.9600 . ? 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 O4 Zn1 O2 139.08(11) 1_556 . ? O4 Zn1 O5 113.50(11) 1_556 2_667 ? O2 Zn1 O5 107.35(11) . 2_667 ? O4 Zn1 O2W 91.10(12) 1_556 . ? O2 Zn1 O2W 92.77(11) . . ? O5 Zn1 O2W 87.75(11) 2_667 . ? O4 Zn1 O1W 91.08(11) 1_556 . ? O2 Zn1 O1W 85.45(11) . . ? O5 Zn1 O1W 91.56(10) 2_667 . ? O2W Zn1 O1W 177.81(10) . . ? O4 Zn1 C1 111.24(12) 1_556 . ? O2 Zn1 C1 28.55(11) . . ? O5 Zn1 C1 135.05(12) 2_667 . ? O2W Zn1 C1 87.34(11) . . ? O1W Zn1 C1 91.69(11) . . ? C1 O2 Zn1 102.9(2) . . ? C7 O3 C9 117.3(3) . . ? C2 O4 Zn1 125.6(2) . 1_554 ? C2 O5 Zn1 138.8(2) . 2_667 ? O1 C1 O2 121.7(3) . . ? O1 C1 C3 120.2(3) . . ? O2 C1 C3 118.1(3) . . ? O1 C1 Zn1 73.5(2) . . ? O2 C1 Zn1 48.52(17) . . ? C3 C1 Zn1 165.9(3) . . ? O4 C2 O5 125.0(3) . . ? O4 C2 C5 116.3(3) . . ? O5 C2 C5 118.8(3) . . ? C8 C3 C4 120.4(3) . . ? C8 C3 C1 119.7(3) . . ? C4 C3 C1 119.9(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 121.0(3) . . ? C6 C5 C2 119.1(3) . . ? C4 C5 C2 119.8(3) . . ? C5 C6 C7 119.1(3) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? O3 C7 C8 116.2(3) . . ? O3 C7 C6 123.6(3) . . ? C8 C7 C6 120.2(3) . . ? C3 C8 C7 120.3(3) . . ? C3 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? O3 C9 C10 108.2(3) . . ? O3 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 C10 C10 110.1(4) . 2_547 ? C9 C10 H10A 109.6 . . ? C10 C10 H10A 109.6 2_547 . ? C9 C10 H10B 109.6 . . ? C10 C10 H10B 109.6 2_547 . ? H10A C10 H10B 108.2 . . ? Zn1 O1W H1WA 120.6 . . ? Zn1 O1W H1WB 135.4 . . ? H1WA O1W H1WB 95.9 . . ? Zn1 O2W H2WA 128.9 . . ? Zn1 O2W H2WB 120.6 . . ? H2WA O2W H2WB 97.2 . . ? H3WA O3W H3WB 111.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3W 0.96 2.18 2.986(4) 140.7 2_668 O1W H1WB O3 0.96 1.90 2.815(4) 157.7 1_565 O2W H2WA O3W 0.96 1.99 2.749(4) 134.9 . O2W H2WB O1 0.96 1.79 2.746(4) 171.3 2_658 O3W H3WA O1W 0.96 1.91 2.830(4) 159.4 1_655 O3W H3WB O1 0.96 2.14 2.964(4) 143.0 1_655 _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 32.87 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 1.081 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.140 # Attachment 'B618796J_compound2.CIF' # Compound 2 data_dl03_0m _database_code_depnum_ccdc_archive 'CCDC 632265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H51 N3 O26 Zn4, H2 O, 3(O)' _chemical_formula_sum 'C49 H59 N3 O30 Zn4' _chemical_formula_weight 1431.47 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0757(6) _cell_length_b 14.1157(7) _cell_length_c 16.6631(8) _cell_angle_alpha 66.6020(10) _cell_angle_beta 87.1380(10) _cell_angle_gamma 89.7570(10) _cell_volume 2818.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6820 _cell_measurement_theta_min 3.74 _cell_measurement_theta_max 32.65 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7174 _exptl_absorpt_correction_T_max 0.9486 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.84600 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'SRS station 16.2smx' _diffrn_radiation_monochromator silicon(111) _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'fine slice \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19414 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 31.00 _reflns_number_total 10334 _reflns_number_gt 8910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0644P)^2^+4.2514P] 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 10334 _refine_ls_number_parameters 782 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 0.76478(3) 0.16630(3) 0.58207(3) 0.01007(12) Uani 1 1 d . . . Zn2 Zn 1.09717(3) 0.53893(3) 0.71826(3) 0.00921(12) Uani 1 1 d . . . Zn3 Zn 1.25292(3) 0.41008(3) 0.87105(3) 0.01348(13) Uani 1 1 d . . . Zn4 Zn 0.59182(3) 0.04083(3) 0.74277(3) 0.01097(12) Uani 1 1 d . . . O1 O 0.6989(2) 0.0576(2) 0.81709(19) 0.0250(7) Uani 1 1 d . . . O2 O 0.7850(2) 0.1777(2) 0.70270(17) 0.0128(6) Uani 1 1 d . . . O3 O 1.0320(2) 0.4001(2) 0.76741(19) 0.0190(6) Uani 1 1 d . . . O4 O 1.1209(2) 0.3260(2) 0.88741(19) 0.0233(7) Uani 1 1 d . . . O5 O 0.8923(3) 0.0348(2) 1.07988(19) 0.0265(8) Uani 1 1 d . . . O21 O 0.6752(2) 0.02046(19) 1.64374(17) 0.0120(6) Uani 1 1 d . . . O22 O 0.6768(3) -0.1229(2) 1.7630(2) 0.0314(8) Uani 1 1 d . . . O23 O 1.0004(2) -0.3760(2) 1.62799(19) 0.0189(6) Uani 1 1 d . . . O24 O 0.9568(2) -0.3706(2) 1.75562(19) 0.0192(6) Uani 1 1 d . . . O25 O 0.7553(2) -0.1299(2) 1.41670(19) 0.0215(7) Uani 1 1 d . . . O41 O 0.5352(2) 0.1791(2) 0.68908(17) 0.0144(6) Uani 1 1 d . . . O42 O 0.6297(2) 0.2454(2) 0.56229(17) 0.0155(6) Uani 1 1 d . . . O43 O 0.2016(2) 0.5170(3) 0.63714(19) 0.0244(7) Uani 1 1 d . . . O44 O 0.2950(2) 0.4185(2) 0.74664(18) 0.0222(7) Uani 1 1 d . . . O45 O 0.3818(2) 0.4939(2) 0.36764(18) 0.0195(6) Uani 1 1 d . . . O46 O 0.2838(3) 0.6720(2) 0.05761(19) 0.0264(7) Uani 1 1 d . . . O47 O 0.16681(19) 0.55145(19) -0.17813(17) 0.0112(5) Uani 1 1 d . . . O48 O 0.1877(2) 0.6928(2) -0.29849(18) 0.0201(6) Uani 1 1 d . . . O49 O 0.4835(2) 0.9565(2) -0.1684(2) 0.0224(7) Uani 1 1 d . . . O50 O 0.4569(2) 0.9481(2) -0.2943(2) 0.0281(8) Uani 1 1 d . . . C1 C 0.7684(3) 0.1257(3) 0.7830(3) 0.0123(8) Uani 1 1 d . . . C2 C 1.0488(3) 0.3284(3) 0.8400(3) 0.0137(8) Uani 1 1 d . . . C3 C 0.8378(3) 0.1436(3) 0.8458(2) 0.0112(8) Uani 1 1 d . . . C4 C 0.9085(3) 0.2241(3) 0.8148(2) 0.0113(8) Uani 1 1 d . . . H4 H 0.9128 0.2689 0.7545 0.014 Uiso 1 1 calc R . . C5 C 0.9738(3) 0.2389(3) 0.8728(3) 0.0121(8) Uani 1 1 d . . . C6 C 0.9676(3) 0.1732(3) 0.9606(3) 0.0164(9) Uani 1 1 d . . . H6 H 1.0131 0.1825 0.9997 0.020 Uiso 1 1 calc R . . C7 C 0.8944(3) 0.0932(3) 0.9917(3) 0.0173(9) Uani 1 1 d . . . C8 C 0.8288(3) 0.0789(3) 0.9344(3) 0.0137(8) Uani 1 1 d . . . H8 H 0.7781 0.0254 0.9554 0.016 Uiso 1 1 calc R . . C9 C 0.8205(3) -0.0494(3) 1.1155(3) 0.0205(9) Uani 1 1 d . . . H9A H 0.8295 -0.0970 1.0853 0.025 Uiso 1 1 calc R . . H9B H 0.7495 -0.0238 1.1089 0.025 Uiso 1 1 calc R . . C10 C 0.8418(3) -0.1029(3) 1.2097(3) 0.0200(9) Uani 1 1 d . . . H10 H 0.9111 -0.1187 1.2236 0.024 Uiso 1 1 calc R . . C21 C 0.6995(3) -0.0750(3) 1.6840(3) 0.0160(8) Uani 1 1 d . . . C22 C 0.9451(3) -0.3414(3) 1.6757(3) 0.0157(9) Uani 1 1 d . . . C23 C 0.7523(3) -0.1300(3) 1.6333(3) 0.0138(8) Uani 1 1 d . . . C24 C 0.8178(3) -0.2096(3) 1.6770(3) 0.0142(8) Uani 1 1 d . . . H24 H 0.8289 -0.2278 1.7371 0.017 Uiso 1 1 calc R . . C25 C 0.8672(3) -0.2625(3) 1.6314(3) 0.0129(8) Uani 1 1 d . . . C26 C 0.8471(3) -0.2392(3) 1.5441(3) 0.0153(8) Uani 1 1 d . . . H26 H 0.8791 -0.2766 1.5137 0.018 Uiso 1 1 calc R . . C27 C 0.7792(3) -0.1600(3) 1.5020(3) 0.0167(9) Uani 1 1 d . . . C28 C 0.7336(3) -0.1045(3) 1.5463(3) 0.0158(8) Uani 1 1 d . . . H28 H 0.6897 -0.0491 1.5169 0.019 Uiso 1 1 calc R . . C29 C 0.7999(3) -0.1861(3) 1.3686(3) 0.0172(9) Uani 1 1 d . . . H29A H 0.7725 -0.2578 1.3925 0.021 Uiso 1 1 calc R . . H29B H 0.8753 -0.1884 1.3726 0.021 Uiso 1 1 calc R . . C30 C 0.7724(3) -0.1304(3) 1.2759(3) 0.0180(9) Uani 1 1 d . . . H30 H 0.7028 -0.1141 0.2639 0.022 Uiso 1 1 calc R . . C41 C 0.5537(3) 0.2443(3) 0.6112(2) 0.0109(8) Uani 1 1 d . . . C42 C 0.2742(3) 0.4557(3) 0.6681(3) 0.0122(8) Uani 1 1 d . . . C43 C 0.4759(3) 0.3273(3) 0.5770(2) 0.0097(7) Uani 1 1 d . . . C44 C 0.4133(3) 0.3518(3) 0.6362(2) 0.0107(8) Uani 1 1 d . . . H44 H 0.4207 0.3170 0.6974 0.013 Uiso 1 1 calc R . . C45 C 0.3401(3) 0.4276(3) 0.6046(3) 0.0109(8) Uani 1 1 d . . . C46 C 0.3262(3) 0.4764(3) 0.5148(3) 0.0133(8) Uani 1 1 d . . . H46 H 0.2747 0.5267 0.4935 0.016 Uiso 1 1 calc R . . C47 C 0.3884(3) 0.4504(3) 0.4572(2) 0.0136(8) Uani 1 1 d . . . C48 C 0.4648(3) 0.3776(3) 0.4880(2) 0.0120(8) Uani 1 1 d . . . H48 H 0.5092 0.3626 0.4478 0.014 Uiso 1 1 calc R . . C49 C 0.2960(3) 0.5609(3) 0.3352(3) 0.0191(9) Uani 1 1 d . . . H49A H 0.3023 0.6231 0.3483 0.023 Uiso 1 1 calc R . . H49B H 0.2310 0.5245 0.3632 0.023 Uiso 1 1 calc R . . C50 C 0.2977(3) 0.5908(3) 0.2383(3) 0.0201(9) Uani 1 1 d . . . H50 H 0.3530 0.6322 0.2026 0.024 Uiso 1 1 calc R . . C51 C 0.2244(3) 0.5613(3) 0.2013(3) 0.0181(9) Uani 1 1 d . . . H51 H 0.1715 0.5185 0.2395 0.022 Uiso 1 1 calc R . . C52 C 0.2157(3) 0.5877(3) 0.1065(3) 0.0203(9) Uani 1 1 d . . . H52A H 0.2333 0.5272 0.0930 0.024 Uiso 1 1 calc R . . H52B H 0.1444 0.6070 0.0902 0.024 Uiso 1 1 calc R . . C53 C 0.2885(3) 0.7053(3) -0.0315(3) 0.0179(9) Uani 1 1 d . . . C54 C 0.2378(3) 0.6579(3) -0.0774(3) 0.0148(8) Uani 1 1 d . . . H54 H 0.1950 0.5989 -0.0469 0.018 Uiso 1 1 calc R . . C55 C 0.2500(3) 0.6973(3) -0.1684(3) 0.0124(8) Uani 1 1 d . . . C56 C 0.3118(3) 0.7844(3) -0.2135(3) 0.0126(8) Uani 1 1 d . . . H56 H 0.3189 0.8117 -0.2756 0.015 Uiso 1 1 calc R . . C57 C 0.3628(3) 0.8311(3) -0.1673(3) 0.0140(8) Uani 1 1 d . . . C58 C 0.3498(3) 0.7922(3) -0.0766(3) 0.0202(9) Uani 1 1 d . . . H58 H 0.3830 0.8255 -0.0452 0.024 Uiso 1 1 calc R . . C59 C 0.1995(3) 0.6462(3) -0.2188(3) 0.0128(8) Uani 1 1 d . . . C60 C 0.4378(3) 0.9183(3) -0.2139(3) 0.0185(9) Uani 1 1 d . . . O1S O 0.8992(2) 0.0809(2) 0.60037(19) 0.0199(6) Uani 1 1 d . . . O2S O 1.3850(2) 0.4897(2) 0.8711(2) 0.0291(8) Uani 1 1 d . . . O3S O 1.3302(3) 0.2703(3) 0.9227(2) 0.0351(9) Uani 1 1 d . . . N1S N 1.0045(3) -0.0448(3) 0.6830(3) 0.0233(8) Uani 1 1 d . . . N2S N 1.5170(3) 0.6018(3) 0.8136(3) 0.0385(12) Uani 1 1 d . . . N3S N 1.4634(5) 0.1646(5) 0.9221(5) 0.0703(18) Uani 1 1 d . . . C1S C 0.9271(3) 0.0189(3) 0.6722(3) 0.0226(10) Uani 1 1 d . . . H1S H 0.8898 0.0169 0.7232 0.027 Uiso 1 1 calc R . . C2S C 1.0280(5) -0.1193(4) 0.7702(4) 0.0421(14) Uani 1 1 d . . . H2S1 H 0.9803 -0.1109 0.8141 0.063 Uiso 1 1 calc R . . H2S2 H 1.0983 -0.1074 0.7824 0.063 Uiso 1 1 calc R . . H2S3 H 1.0212 -0.1895 0.7726 0.063 Uiso 1 1 calc R . . C3S C 1.0645(4) -0.0504(4) 0.6100(4) 0.0338(12) Uani 1 1 d . . . H3S1 H 1.0481 -0.1150 0.6042 0.051 Uiso 1 1 calc R . . H3S2 H 1.1376 -0.0483 0.6201 0.051 Uiso 1 1 calc R . . H3S3 H 1.0487 0.0082 0.5562 0.051 Uiso 1 1 calc R . . C4S C 1.4401(4) 0.5431(4) 0.8096(4) 0.0375(13) Uani 1 1 d . . . H4S H 1.4274 0.5430 0.7540 0.045 Uiso 1 1 calc R . . C5S C 1.5751(7) 0.6659(6) 0.7351(5) 0.085(3) Uani 1 1 d . . . H5S1 H 1.5628 0.6426 0.6883 0.128 Uiso 1 1 calc R . . H5S2 H 1.6482 0.6610 0.7463 0.128 Uiso 1 1 calc R . . H5S3 H 1.5538 0.7377 0.7173 0.128 Uiso 1 1 calc R . . C6S C 1.5409(6) 0.6117(6) 0.8944(5) 0.077(2) Uani 1 1 d . . . H6S1 H 1.4834 0.5843 0.9377 0.115 Uiso 1 1 calc R . . H6S2 H 1.5526 0.6846 0.8826 0.115 Uiso 1 1 calc R . . H6S3 H 1.6027 0.5728 0.9173 0.115 Uiso 1 1 calc R . . C7S C 1.4294(7) 0.2627(5) 0.8999(4) 0.060(2) Uani 1 1 d . . . H7S H 1.4726 0.3216 0.8703 0.072 Uiso 1 1 calc R . . C8S C 1.5483(17) 0.1578(13) 0.8882(11) 0.253(12) Uani 1 1 d . . . H8S1 H 1.5398 0.1605 0.8292 0.380 Uiso 1 1 calc R . . H8S2 H 1.5795 0.0922 0.9240 0.380 Uiso 1 1 calc R . . H8S3 H 1.5928 0.2152 0.8846 0.380 Uiso 1 1 calc R . . C9S C 1.4153(14) 0.0813(14) 1.0005(10) 0.221(9) Uani 1 1 d . . . H9S1 H 1.3862 0.0284 0.9836 0.331 Uiso 1 1 calc R . . H9S2 H 1.3608 0.1100 1.0261 0.331 Uiso 1 1 calc R . . H9S3 H 1.4671 0.0503 1.0435 0.331 Uiso 1 1 calc R . . O1W O 0.8495(2) 0.3035(2) 0.5215(2) 0.0231(7) Uani 1 1 d . . . H1WA H 0.9072 0.3002 0.4848 0.028 Uiso 1 1 d R . . H1WB H 0.8275 0.3534 0.4669 0.028 Uiso 1 1 d R . . O2W O 0.7469(2) 0.1566(2) 0.46238(17) 0.0152(6) Uani 1 1 d . . . H2WA H 0.6774 0.1374 0.4589 0.018 Uiso 1 1 d R . . H2WB H 0.7604 0.2127 0.4067 0.018 Uiso 1 1 d R . . O3W O 1.2224(3) 0.3884(3) 1.0034(2) 0.0417(9) Uani 1 1 d . . . H3WA H 1.1598 0.4166 1.0163 0.050 Uiso 1 1 d R . . H3WB H 1.2253 0.3179 1.0447 0.050 Uiso 1 1 d R . . O4W O 0.4444(3) 0.9021(3) 0.5629(2) 0.0426(10) Uani 1 1 d . . . H4WA H 0.4558 0.8776 0.6242 0.051 Uiso 1 1 d R . . H4WB H 0.5037 0.9418 0.5313 0.051 Uiso 1 1 d R . . O5W O 0.0377(6) 0.4432(9) 0.0569(6) 0.058(3) Uiso 0.58(2) 1 d P A 1 O5W' O 0.0438(8) 0.3789(12) 0.0756(8) 0.055(4) Uiso 0.42(2) 1 d P A 2 O6W O 0.7394(5) 0.8378(5) 0.9158(4) 0.039(2) Uiso 0.592(11) 1 d P B 1 O6W' O 0.8147(7) 0.8104(7) 0.9085(6) 0.039(3) Uiso 0.408(11) 1 d P B 2 O7W O 0.0482(14) 0.4179(12) 0.5532(11) 0.046(6) Uiso 0.282(19) 1 d P C 1 O7W' O -0.0096(8) 0.3989(6) 0.5859(6) 0.081(3) Uiso 0.718(19) 1 d P C 2 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 0.0097(2) 0.0102(2) 0.0064(2) 0.00055(18) 0.00129(16) 0.00020(17) Zn2 0.0089(2) 0.0104(2) 0.0073(2) -0.00243(18) 0.00009(16) -0.00031(17) Zn3 0.0116(2) 0.0157(2) 0.0105(2) -0.00241(19) -0.00017(17) -0.00400(18) Zn4 0.0097(2) 0.0114(2) 0.0075(2) 0.00072(18) 0.00119(17) -0.00111(17) O1 0.0172(16) 0.0297(17) 0.0145(15) 0.0064(13) -0.0067(12) -0.0155(13) O2 0.0163(14) 0.0120(13) 0.0081(14) -0.0018(11) -0.0005(11) -0.0039(11) O3 0.0174(15) 0.0132(14) 0.0215(16) -0.0006(12) -0.0097(12) -0.0048(11) O4 0.0204(16) 0.0229(16) 0.0159(15) 0.0046(13) -0.0076(12) -0.0127(13) O5 0.042(2) 0.0236(16) 0.0087(15) 0.0001(13) -0.0066(13) -0.0186(14) O21 0.0118(14) 0.0078(13) 0.0130(14) -0.0007(11) 0.0011(11) -0.0001(10) O22 0.044(2) 0.0192(16) 0.0188(17) 0.0035(14) 0.0132(15) 0.0098(15) O23 0.0185(15) 0.0169(15) 0.0237(16) -0.0100(13) -0.0087(12) 0.0095(12) O24 0.0186(15) 0.0168(15) 0.0160(16) 0.0006(12) -0.0062(12) 0.0035(12) O25 0.0292(17) 0.0189(15) 0.0150(15) -0.0047(13) -0.0078(13) 0.0085(13) O41 0.0180(15) 0.0129(14) 0.0095(14) -0.0020(11) 0.0016(11) 0.0041(11) O42 0.0150(14) 0.0177(14) 0.0105(14) -0.0024(12) 0.0020(11) 0.0088(11) O43 0.0186(16) 0.0410(19) 0.0138(15) -0.0113(14) -0.0017(12) 0.0176(14) O44 0.0244(16) 0.0311(17) 0.0089(15) -0.0060(13) 0.0030(12) 0.0124(13) O45 0.0237(16) 0.0249(16) 0.0078(14) -0.0040(12) -0.0053(12) 0.0114(13) O46 0.0394(19) 0.0242(16) 0.0099(15) -0.0002(13) -0.0031(13) -0.0200(14) O47 0.0098(13) 0.0101(13) 0.0124(14) -0.0033(11) 0.0006(10) -0.0032(10) O48 0.0240(16) 0.0245(16) 0.0093(15) -0.0043(13) 0.0034(12) -0.0119(13) O49 0.0174(15) 0.0168(15) 0.0344(18) -0.0127(14) 0.0068(13) -0.0104(12) O50 0.0207(17) 0.0279(17) 0.0217(18) 0.0050(14) -0.0007(13) -0.0160(13) C1 0.0103(19) 0.0116(19) 0.013(2) -0.0020(16) -0.0030(15) 0.0019(15) C2 0.014(2) 0.014(2) 0.014(2) -0.0068(17) 0.0013(16) -0.0042(16) C3 0.0105(19) 0.0120(18) 0.0105(19) -0.0040(16) -0.0001(15) -0.0006(15) C4 0.0114(19) 0.0097(18) 0.0112(19) -0.0023(15) -0.0013(15) 0.0003(15) C5 0.0116(19) 0.0092(18) 0.013(2) -0.0016(15) 0.0005(15) -0.0036(15) C6 0.018(2) 0.016(2) 0.015(2) -0.0061(17) -0.0047(16) -0.0069(16) C7 0.024(2) 0.015(2) 0.0083(19) -0.0003(16) -0.0017(16) -0.0027(17) C8 0.016(2) 0.0106(19) 0.011(2) -0.0006(16) 0.0008(15) -0.0047(15) C9 0.027(2) 0.017(2) 0.012(2) -0.0002(17) 0.0006(17) -0.0086(18) C10 0.026(2) 0.016(2) 0.015(2) -0.0022(17) -0.0044(18) -0.0033(18) C21 0.014(2) 0.015(2) 0.014(2) -0.0001(17) 0.0025(16) -0.0006(16) C22 0.0102(19) 0.0087(18) 0.023(2) -0.0014(17) 0.0002(16) -0.0049(15) C23 0.0103(19) 0.0103(19) 0.017(2) -0.0017(16) 0.0036(15) -0.0019(15) C24 0.014(2) 0.0133(19) 0.012(2) -0.0016(16) -0.0013(15) -0.0001(16) C25 0.0098(19) 0.0094(18) 0.015(2) -0.0002(16) -0.0021(15) -0.0010(15) C26 0.020(2) 0.0083(18) 0.015(2) -0.0019(16) -0.0011(16) -0.0009(16) C27 0.019(2) 0.0121(19) 0.012(2) 0.0028(16) -0.0041(16) 0.0002(16) C28 0.015(2) 0.0089(18) 0.017(2) 0.0020(16) -0.0015(16) -0.0009(15) C29 0.023(2) 0.014(2) 0.012(2) -0.0035(17) -0.0006(17) -0.0021(17) C30 0.022(2) 0.014(2) 0.015(2) -0.0017(17) -0.0028(17) -0.0045(17) C41 0.014(2) 0.0109(18) 0.0090(19) -0.0050(16) -0.0030(15) 0.0005(15) C42 0.0099(19) 0.0141(19) 0.013(2) -0.0064(16) -0.0014(15) 0.0006(15) C43 0.0067(18) 0.0096(18) 0.0109(19) -0.0023(15) 0.0008(14) -0.0014(14) C44 0.0103(19) 0.0143(19) 0.0060(18) -0.0025(15) -0.0002(14) -0.0006(15) C45 0.0088(18) 0.0109(18) 0.014(2) -0.0061(16) 0.0022(15) -0.0024(14) C46 0.0112(19) 0.0121(19) 0.016(2) -0.0044(16) -0.0030(15) 0.0014(15) C47 0.018(2) 0.0138(19) 0.0066(18) -0.0015(16) -0.0020(15) -0.0008(16) C48 0.0135(19) 0.0139(19) 0.0095(19) -0.0060(16) 0.0030(15) -0.0005(15) C49 0.020(2) 0.023(2) 0.013(2) -0.0058(18) -0.0065(17) 0.0072(18) C50 0.021(2) 0.020(2) 0.012(2) 0.0014(17) -0.0026(17) -0.0003(17) C51 0.020(2) 0.017(2) 0.016(2) -0.0053(17) 0.0018(17) -0.0029(17) C52 0.027(2) 0.017(2) 0.015(2) -0.0043(18) -0.0006(18) -0.0093(18) C53 0.023(2) 0.016(2) 0.012(2) -0.0020(17) -0.0029(16) -0.0063(17) C54 0.015(2) 0.0113(19) 0.014(2) -0.0006(16) 0.0029(16) -0.0073(15) C55 0.0116(19) 0.0123(19) 0.0117(19) -0.0030(16) -0.0014(15) -0.0009(15) C56 0.0109(19) 0.0143(19) 0.0088(19) -0.0006(16) -0.0002(15) -0.0011(15) C57 0.0120(19) 0.0096(18) 0.017(2) -0.0019(16) -0.0006(16) -0.0048(15) C58 0.024(2) 0.016(2) 0.019(2) -0.0047(18) -0.0084(18) -0.0100(17) C59 0.0094(19) 0.015(2) 0.014(2) -0.0061(17) 0.0026(15) -0.0012(15) C60 0.010(2) 0.011(2) 0.027(3) -0.0002(18) -0.0020(17) -0.0020(16) O1S 0.0138(15) 0.0218(15) 0.0211(16) -0.0053(13) -0.0017(12) 0.0028(12) O2S 0.0133(16) 0.0257(17) 0.043(2) -0.0084(16) -0.0010(14) -0.0056(13) O3S 0.031(2) 0.0242(18) 0.041(2) -0.0015(16) -0.0166(16) 0.0031(15) N1S 0.0171(19) 0.024(2) 0.036(2) -0.0191(18) -0.0101(16) 0.0076(15) N2S 0.018(2) 0.025(2) 0.075(4) -0.025(2) 0.017(2) -0.0102(17) N3S 0.076(5) 0.064(4) 0.062(4) -0.014(3) -0.025(3) -0.013(3) C1S 0.023(2) 0.023(2) 0.023(2) -0.010(2) -0.0034(18) 0.0068(19) C2S 0.056(4) 0.041(3) 0.039(3) -0.023(3) -0.028(3) 0.026(3) C3S 0.020(2) 0.029(3) 0.052(3) -0.017(2) 0.007(2) 0.002(2) C4S 0.036(3) 0.033(3) 0.048(3) -0.023(3) 0.016(3) -0.012(2) C5S 0.098(6) 0.073(5) 0.107(7) -0.068(5) 0.068(5) -0.061(5) C6S 0.059(5) 0.075(5) 0.080(6) -0.010(4) -0.029(4) -0.025(4) C7S 0.122(7) 0.029(3) 0.029(3) -0.012(3) -0.005(4) 0.024(4) C8S 0.41(3) 0.156(15) 0.186(17) -0.079(13) 0.15(2) 0.015(18) C9S 0.26(2) 0.24(2) 0.127(13) -0.031(14) 0.014(14) 0.025(17) O1W 0.0217(16) 0.0199(16) 0.0197(16) 0.0000(13) 0.0034(13) -0.0072(13) O2W 0.0164(15) 0.0194(15) 0.0076(14) -0.0033(12) 0.0017(11) 0.0008(11) O3W 0.042(2) 0.064(3) 0.0183(18) -0.0153(18) -0.0051(16) 0.0084(19) O4W 0.032(2) 0.064(3) 0.0222(19) -0.0071(18) -0.0013(15) -0.0129(18) _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 O42 2.055(3) . ? Zn1 O2W 2.077(3) . ? Zn1 O1W 2.085(3) . ? Zn1 O1S 2.093(3) . ? Zn1 O2 2.109(3) . ? Zn1 O21 2.210(3) . ? Zn2 O3 1.976(3) . ? Zn2 O43 1.983(3) 1_655 ? Zn2 O23 2.012(3) 1_565 ? Zn2 O47 2.059(3) 1_656 ? Zn2 O48 2.389(3) 1_656 ? Zn2 O24 2.426(3) 1_565 ? Zn2 C22 2.544(4) 1_565 ? Zn2 C59 2.569(4) 1_656 ? Zn3 O4 2.043(3) . ? Zn3 O2S 2.065(3) . ? Zn3 O44 2.075(3) 1_655 ? Zn3 O3S 2.092(3) . ? Zn3 O3W 2.120(3) . ? Zn3 O47 2.167(3) 1_656 ? Zn4 O41 1.956(3) . ? Zn4 O1 1.990(3) . ? Zn4 O49 2.005(3) 1_546 ? Zn4 O21 2.047(3) . ? Zn4 O50 2.446(3) 1_546 ? Zn4 O22 2.467(3) . ? Zn4 C60 2.542(4) 1_546 ? O1 C1 1.263(5) . ? O2 C1 1.253(5) . ? O3 C2 1.260(5) . ? O4 C2 1.252(5) . ? O5 C7 1.369(5) . ? O5 C9 1.429(5) . ? O21 C21 1.290(5) . ? O22 C21 1.238(5) . ? O23 C22 1.280(5) . ? O23 Zn2 2.012(3) 1_545 ? O24 C22 1.245(5) . ? O24 Zn2 2.426(3) 1_545 ? O25 C27 1.364(5) . ? O25 C29 1.437(5) . ? O41 C41 1.270(5) . ? O42 C41 1.248(5) . ? O43 C42 1.266(5) . ? O43 Zn2 1.983(3) 1_455 ? O44 C42 1.246(5) . ? O44 Zn3 2.075(3) 1_455 ? O45 C47 1.377(5) . ? O45 C49 1.446(5) . ? O46 C53 1.365(5) . ? O46 C52 1.428(5) . ? O47 C59 1.299(5) . ? O47 Zn2 2.059(3) 1_454 ? O47 Zn3 2.167(3) 1_454 ? O48 C59 1.243(5) . ? O48 Zn2 2.389(3) 1_454 ? O49 C60 1.263(5) . ? O49 Zn4 2.005(3) 1_564 ? O50 C60 1.247(5) . ? O50 Zn4 2.446(3) 1_564 ? C1 C3 1.512(5) . ? C2 C5 1.506(5) . ? C3 C4 1.382(5) . ? C3 C8 1.392(5) . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C6 C7 1.398(6) . ? C6 H6 0.9500 . ? C7 C8 1.388(6) . ? C8 H8 0.9500 . ? C9 C10 1.488(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C30 1.324(6) 1_556 ? C10 H10 0.9500 . ? C21 C23 1.501(6) . ? C22 C25 1.495(5) . ? C22 Zn2 2.544(4) 1_545 ? C23 C28 1.382(6) . ? C23 C24 1.390(5) . ? C24 C25 1.395(6) . ? C24 H24 0.9500 . ? C25 C26 1.397(6) . ? C26 C27 1.400(5) . ? C26 H26 0.9500 . ? C27 C28 1.387(6) . ? C28 H28 0.9500 . ? C29 C30 1.491(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C10 1.324(6) 1_554 ? C30 H30 0.9500 . ? C41 C43 1.500(5) . ? C42 C45 1.503(5) . ? C43 C48 1.382(5) . ? C43 C44 1.397(5) . ? C44 C45 1.390(5) . ? C44 H44 0.9500 . ? C45 C46 1.398(5) . ? C46 C47 1.385(6) . ? C46 H46 0.9500 . ? C47 C48 1.392(5) . ? C48 H48 0.9500 . ? C49 C50 1.496(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.319(6) . ? C50 H50 0.9500 . ? C51 C52 1.483(6) . ? C51 H51 0.9500 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C58 1.389(6) . ? C53 C54 1.392(6) . ? C54 C55 1.392(5) . ? C54 H54 0.9500 . ? C55 C56 1.393(5) . ? C55 C59 1.484(5) . ? C56 C57 1.389(5) . ? C56 H56 0.9500 . ? C57 C58 1.390(6) . ? C57 C60 1.501(5) . ? C58 H58 0.9500 . ? C59 Zn2 2.569(4) 1_454 ? C60 Zn4 2.542(4) 1_564 ? O1S C1S 1.241(5) . ? O2S C4S 1.206(6) . ? O3S C7S 1.350(8) . ? N1S C1S 1.322(5) . ? N1S C3S 1.443(6) . ? N1S C2S 1.463(6) . ? N2S C4S 1.327(6) . ? N2S C5S 1.439(8) . ? N2S C6S 1.456(9) . ? N3S C8S 1.242(17) . ? N3S C7S 1.362(9) . ? N3S C9S 1.479(16) . ? C1S H1S 0.9500 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C4S H4S 0.9500 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? C7S H7S 0.9500 . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? C9S H9S1 0.9800 . ? C9S H9S2 0.9800 . ? C9S H9S3 0.9800 . ? O1W H1WA 0.9599 . ? O1W H1WB 0.9600 . ? O2W H2WA 0.9600 . ? O2W H2WB 0.9600 . ? O3W H3WA 0.9600 . ? O3W H3WB 0.9600 . ? O4W H4WA 0.9599 . ? O4W H4WB 0.9601 . ? 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 O42 Zn1 O2W 86.89(11) . . ? O42 Zn1 O1W 91.36(12) . . ? O2W Zn1 O1W 91.22(12) . . ? O42 Zn1 O1S 177.39(12) . . ? O2W Zn1 O1S 91.26(11) . . ? O1W Zn1 O1S 90.52(12) . . ? O42 Zn1 O2 93.47(11) . . ? O2W Zn1 O2 179.09(11) . . ? O1W Zn1 O2 87.93(11) . . ? O1S Zn1 O2 88.41(11) . . ? O42 Zn1 O21 88.79(10) . . ? O2W Zn1 O21 87.64(10) . . ? O1W Zn1 O21 178.84(11) . . ? O1S Zn1 O21 89.30(10) . . ? O2 Zn1 O21 93.21(10) . . ? O3 Zn2 O43 98.97(14) . 1_655 ? O3 Zn2 O23 103.49(12) . 1_565 ? O43 Zn2 O23 97.71(12) 1_655 1_565 ? O3 Zn2 O47 104.78(11) . 1_656 ? O43 Zn2 O47 109.97(11) 1_655 1_656 ? O23 Zn2 O47 136.23(11) 1_565 1_656 ? O3 Zn2 O48 163.55(11) . 1_656 ? O43 Zn2 O48 88.76(12) 1_655 1_656 ? O23 Zn2 O48 89.70(11) 1_565 1_656 ? O47 Zn2 O48 58.81(10) 1_656 1_656 ? O3 Zn2 O24 97.03(11) . 1_565 ? O43 Zn2 O24 154.15(11) 1_655 1_565 ? O23 Zn2 O24 58.68(11) 1_565 1_565 ? O47 Zn2 O24 85.17(10) 1_656 1_565 ? O48 Zn2 O24 81.31(10) 1_656 1_565 ? O3 Zn2 C22 103.06(12) . 1_565 ? O43 Zn2 C22 126.50(13) 1_655 1_565 ? O23 Zn2 C22 29.84(13) 1_565 1_565 ? O47 Zn2 C22 110.41(12) 1_656 1_565 ? O48 Zn2 C22 83.46(11) 1_656 1_565 ? O24 Zn2 C22 28.90(12) 1_565 1_565 ? O3 Zn2 C59 134.81(12) . 1_656 ? O43 Zn2 C59 101.45(13) 1_655 1_656 ? O23 Zn2 C59 113.03(12) 1_565 1_656 ? O47 Zn2 C59 30.11(11) 1_656 1_656 ? O48 Zn2 C59 28.74(11) 1_656 1_656 ? O24 Zn2 C59 80.98(11) 1_565 1_656 ? C22 Zn2 C59 96.35(12) 1_565 1_656 ? O4 Zn3 O2S 172.91(13) . . ? O4 Zn3 O44 96.54(13) . 1_655 ? O2S Zn3 O44 90.25(14) . 1_655 ? O4 Zn3 O3S 87.84(13) . . ? O2S Zn3 O3S 90.32(13) . . ? O44 Zn3 O3S 88.46(13) 1_655 . ? O4 Zn3 O3W 84.83(14) . . ? O2S Zn3 O3W 88.20(15) . . ? O44 Zn3 O3W 173.57(13) 1_655 . ? O3S Zn3 O3W 85.30(15) . . ? O4 Zn3 O47 89.99(11) . 1_656 ? O2S Zn3 O47 91.64(11) . 1_656 ? O44 Zn3 O47 93.40(11) 1_655 1_656 ? O3S Zn3 O47 177.29(12) . 1_656 ? O3W Zn3 O47 92.89(13) . 1_656 ? O41 Zn4 O1 103.41(13) . . ? O41 Zn4 O49 105.23(12) . 1_546 ? O1 Zn4 O49 102.58(12) . 1_546 ? O41 Zn4 O21 105.16(11) . . ? O1 Zn4 O21 103.22(12) . . ? O49 Zn4 O21 133.80(11) 1_546 . ? O41 Zn4 O50 97.45(11) . 1_546 ? O1 Zn4 O50 155.00(11) . 1_546 ? O49 Zn4 O50 58.05(11) 1_546 1_546 ? O21 Zn4 O50 84.16(11) . 1_546 ? O41 Zn4 O22 162.36(11) . . ? O1 Zn4 O22 85.33(13) . . ? O49 Zn4 O22 87.38(11) 1_546 . ? O21 Zn4 O22 57.53(10) . . ? O50 Zn4 O22 78.56(12) 1_546 . ? O41 Zn4 C60 105.25(12) . 1_546 ? O1 Zn4 C60 129.30(13) . 1_546 ? O49 Zn4 C60 29.34(13) 1_546 1_546 ? O21 Zn4 C60 108.36(13) . 1_546 ? O50 Zn4 C60 28.88(12) 1_546 1_546 ? O22 Zn4 C60 79.64(12) . 1_546 ? C1 O1 Zn4 119.6(2) . . ? C1 O2 Zn1 139.5(2) . . ? C2 O3 Zn2 126.3(3) . . ? C2 O4 Zn3 135.0(3) . . ? C7 O5 C9 118.1(3) . . ? C21 O21 Zn4 99.5(2) . . ? C21 O21 Zn1 133.8(2) . . ? Zn4 O21 Zn1 102.83(11) . . ? C21 O22 Zn4 81.6(2) . . ? C22 O23 Zn2 98.7(2) . 1_545 ? C22 O24 Zn2 80.8(2) . 1_545 ? C27 O25 C29 117.5(3) . . ? C41 O41 Zn4 126.6(2) . . ? C41 O42 Zn1 133.7(2) . . ? C42 O43 Zn2 119.4(3) . 1_455 ? C42 O44 Zn3 145.4(3) . 1_455 ? C47 O45 C49 116.1(3) . . ? C53 O46 C52 117.6(3) . . ? C59 O47 Zn2 97.2(2) . 1_454 ? C59 O47 Zn3 129.5(2) . 1_454 ? Zn2 O47 Zn3 101.69(11) 1_454 1_454 ? C59 O48 Zn2 83.7(2) . 1_454 ? C60 O49 Zn4 99.6(3) . 1_564 ? C60 O50 Zn4 79.8(2) . 1_564 ? O2 C1 O1 125.7(4) . . ? O2 C1 C3 118.1(3) . . ? O1 C1 C3 116.2(3) . . ? O4 C2 O3 125.9(4) . . ? O4 C2 C5 117.5(3) . . ? O3 C2 C5 116.5(3) . . ? C4 C3 C8 120.9(4) . . ? C4 C3 C1 119.7(3) . . ? C8 C3 C1 119.4(3) . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 C2 120.1(3) . . ? C4 C5 C2 119.7(3) . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? O5 C7 C8 124.6(4) . . ? O5 C7 C6 115.5(3) . . ? C8 C7 C6 120.0(4) . . ? C7 C8 C3 119.5(4) . . ? C7 C8 H8 120.3 . . ? C3 C8 H8 120.3 . . ? O5 C9 C10 105.9(3) . . ? O5 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O5 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? C30 C10 C9 125.6(4) 1_556 . ? C30 C10 H10 117.2 1_556 . ? C9 C10 H10 117.2 . . ? O22 C21 O21 121.2(4) . . ? O22 C21 C23 119.5(4) . . ? O21 C21 C23 119.3(3) . . ? O24 C22 O23 121.6(4) . . ? O24 C22 C25 121.0(4) . . ? O23 C22 C25 117.5(4) . . ? O24 C22 Zn2 70.3(2) . 1_545 ? O23 C22 Zn2 51.45(19) . 1_545 ? C25 C22 Zn2 167.6(3) . 1_545 ? C28 C23 C24 120.8(4) . . ? C28 C23 C21 120.9(4) . . ? C24 C23 C21 118.2(4) . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 C22 119.4(4) . . ? C26 C25 C22 120.2(4) . . ? C25 C26 C27 119.3(4) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? O25 C27 C28 115.7(3) . . ? O25 C27 C26 124.1(4) . . ? C28 C27 C26 120.2(4) . . ? C23 C28 C27 119.9(4) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? O25 C29 C30 106.7(3) . . ? O25 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O25 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C10 C30 C29 122.2(4) 1_554 . ? C10 C30 H30 118.9 1_554 . ? C29 C30 H30 118.9 . . ? O42 C41 O41 126.2(3) . . ? O42 C41 C43 118.5(3) . . ? O41 C41 C43 115.3(3) . . ? O44 C42 O43 124.6(4) . . ? O44 C42 C45 118.4(3) . . ? O43 C42 C45 117.1(3) . . ? C48 C43 C44 120.3(3) . . ? C48 C43 C41 120.4(3) . . ? C44 C43 C41 119.3(3) . . ? C45 C44 C43 119.2(3) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 C42 119.3(3) . . ? C46 C45 C42 119.9(3) . . ? C47 C46 C45 119.1(3) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? O45 C47 C46 123.9(3) . . ? O45 C47 C48 115.4(3) . . ? C46 C47 C48 120.6(3) . . ? C43 C48 C47 119.9(3) . . ? C43 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? O45 C49 C50 107.2(3) . . ? O45 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? O45 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? C51 C50 C49 121.7(4) . . ? C51 C50 H50 119.1 . . ? C49 C50 H50 119.1 . . ? C50 C51 C52 127.0(4) . . ? C50 C51 H51 116.5 . . ? C52 C51 H51 116.5 . . ? O46 C52 C51 109.2(3) . . ? O46 C52 H52A 109.8 . . ? C51 C52 H52A 109.8 . . ? O46 C52 H52B 109.8 . . ? C51 C52 H52B 109.8 . . ? H52A C52 H52B 108.3 . . ? O46 C53 C58 115.6(4) . . ? O46 C53 C54 124.6(4) . . ? C58 C53 C54 119.8(4) . . ? C53 C54 C55 119.6(4) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 120.4(4) . . ? C54 C55 C59 120.7(3) . . ? C56 C55 C59 118.9(3) . . ? C57 C56 C55 119.8(4) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C58 119.7(4) . . ? C56 C57 C60 120.6(4) . . ? C58 C57 C60 119.6(4) . . ? C53 C58 C57 120.6(4) . . ? C53 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? O48 C59 O47 120.1(3) . . ? O48 C59 C55 121.1(3) . . ? O47 C59 C55 118.8(3) . . ? O48 C59 Zn2 67.5(2) . 1_454 ? O47 C59 Zn2 52.68(18) . 1_454 ? C55 C59 Zn2 170.5(3) . 1_454 ? O50 C60 O49 121.8(4) . . ? O50 C60 C57 120.3(4) . . ? O49 C60 C57 117.8(4) . . ? O50 C60 Zn4 71.3(2) . 1_564 ? O49 C60 Zn4 51.0(2) . 1_564 ? C57 C60 Zn4 164.8(3) . 1_564 ? C1S O1S Zn1 124.9(3) . . ? C4S O2S Zn3 128.6(4) . . ? C7S O3S Zn3 121.7(3) . . ? C1S N1S C3S 122.2(4) . . ? C1S N1S C2S 121.0(4) . . ? C3S N1S C2S 116.6(4) . . ? C4S N2S C5S 120.3(6) . . ? C4S N2S C6S 122.4(5) . . ? C5S N2S C6S 117.1(5) . . ? C8S N3S C7S 115.0(10) . . ? C8S N3S C9S 123.9(12) . . ? C7S N3S C9S 118.5(10) . . ? O1S C1S N1S 125.0(4) . . ? O1S C1S H1S 117.5 . . ? N1S C1S H1S 117.5 . . ? N1S C2S H2S1 109.5 . . ? N1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N1S C3S H3S1 109.5 . . ? N1S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? N1S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? O2S C4S N2S 125.1(6) . . ? O2S C4S H4S 117.5 . . ? N2S C4S H4S 117.5 . . ? N2S C5S H5S1 109.5 . . ? N2S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? N2S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? N2S C6S H6S1 109.5 . . ? N2S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? N2S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? O3S C7S N3S 115.3(7) . . ? O3S C7S H7S 122.4 . . ? N3S C7S H7S 122.4 . . ? N3S C8S H8S1 109.5 . . ? N3S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? N3S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? N3S C9S H9S1 109.5 . . ? N3S C9S H9S2 109.5 . . ? H9S1 C9S H9S2 109.5 . . ? N3S C9S H9S3 109.5 . . ? H9S1 C9S H9S3 109.5 . . ? H9S2 C9S H9S3 109.5 . . ? Zn1 O1W H1WA 115.0 . . ? Zn1 O1W H1WB 118.2 . . ? H1WA O1W H1WB 82.0 . . ? Zn1 O2W H2WA 109.8 . . ? Zn1 O2W H2WB 124.1 . . ? H2WA O2W H2WB 102.6 . . ? Zn3 O3W H3WA 116.4 . . ? Zn3 O3W H3WB 114.5 . . ? H3WA O3W H3WB 107.7 . . ? H4WA O4W H4WB 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O23 0.96 2.08 2.934(4) 147.4 2_756 O1W H1WB O43 0.96 2.01 2.949(4) 165.5 2_666 O2W H2WA O4W 0.96 1.79 2.741(4) 170.6 2_666 O2W H2WB O48 0.96 1.86 2.807(4) 167.8 2_665 O3W H3WA O5W' 0.96 1.73 2.552(11) 141.1 1_656 O3W H3WA O5W 0.96 1.80 2.746(10) 168.2 1_656 O3W H3WB O6W' 0.96 1.73 2.632(10) 154.3 2_767 O3W H3WB O6W 0.96 2.09 2.982(7) 154.6 2_767 O4W H4WA O50 0.96 1.98 2.716(5) 132.2 1_556 O4W H4WB O4W 0.96 2.22 3.046(7) 143.2 2_676 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.338 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.121 # Attachment 'B618796J_compound3.cif' # CIF-file generated for #============================================================================== data_sh541 _database_code_depnum_ccdc_archive 'CCDC 632266' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 O10 Zn2, 4O' _chemical_formula_sum 'C20 H20 O14 Zn2' _chemical_formula_weight 303.54 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.5471(7) _cell_length_b 7.8520(7) _cell_length_c 8.4756(6) _cell_angle_alpha 91.891(4) _cell_angle_beta 107.086(3) _cell_angle_gamma 100.815(4) _cell_volume 593.90(8) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 18 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ; _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 3.139 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 12 # perpendicular to equatorial plane _pd_spec_size_equat 1.0 # parallel to scattering vector in transmission _pd_spec_size_thick 1.0 # parallel to scattering vector in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting '1.0 mm borosilicate capillary' _pd_spec_mount_mode transmission _pd_spec_shape cylinder _pd_char_particle_morphology ? _pd_char_colour white # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_temperature 298 _exptl_absorpt_correction_type ' none' #=============================================================================== # 7. EXPERIMENTAL DATA # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location 'Solid-State Research Group, University of Strathclyde, Glasgow, U.K.' _diffrn_ambient_temperature 298 _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Cu K\a~1~' # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 1.54056 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Bruker-AXS D8' _diffrn_source_target Cu _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_radiation_monochromator 'primary focussing, Ge 111' _diffrn_detector Bruker-Vantec _diffrn_detector_type 'Solid state detector' _pd_meas_scan_method step _pd_meas_special_details ; Data were collected using a variable count time (VCT) scheme in which the step time is increased with 2\q (Shankland et al., 1997; Hill & Madsen, 2002). The specific scheme used was: Data Ranges / \% 2\q Step Times in Each Range (s) 3 - 43.0 5 43.0 - 65.0 20 ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 3647 _pd_meas_2theta_range_min 3.0 _pd_meas_2theta_range_max 65.0 _pd_meas_2theta_range_inc 0.017 # The following fields are used to identify the programs used. _computing_data_collection 'DIFFRAC plus XRD Commander (Kienle & Jacob, 2003)' _computing_data_reduction 'DASH (David et al., 2001)' _computing_structure_solution 'DASH (David et al., 2001)' _computing_structure_refinement 'TOPAS (Coelho, 2003)' _computing_publication_material 'enCifer (Cambridge Crystallographic Data Centre, 2004)' _computing_cell_refinement 'TOPAS (Coelho, 2003)' _computing_molecular_graphics 'Mercury (Macrae et al., 2006)' #=============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. # The next three items are given as text. _pd_proc_ls_profile_function ; Fundamental parameters with axial divergence correction. ; _pd_proc_ls_background_function ; Chebyshev polynomial ; _pd_proc_ls_pref_orient_corr ; A spherical harmonics-based preferred orientation correction (J\"arvinen, 1993) was applied with Topas during the Rietveld refinement. ; _pd_proc_ls_prof_R_factor 0.0478 _pd_proc_ls_prof_wR_factor 0.0630 _pd_proc_ls_prof_wR_expected 0.0164 _refine_ls_matrix_type sparse _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 1/\s(Y~obs~)^2^ _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 95 _refine_ls_number_restraints 57 _refine_ls_number_constraints 1 _refine_diff_density_max 0.2 _refine_diff_density_min -0.2 _refine_ls_shift/su_max 0.001 _refine_ls_R_I_factor 1.585 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 3.853 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Zn1 Zn Uiso 0.3952(6) 0.4919(7) 0.1632(7) 1.000 0.0435 . . O1 O Uiso -0.2094(5) -0.43347(13) 0.7960(4) 1.000 0.0442 . . O2 O Uiso -0.330(4) -0.34129(12) 0.5599(5) 1.000 0.0442 . . O3 O Uiso 0.108(3) -0.1279(3) 0.3019(3) 1.000 0.0442 . . O4 O Uiso 0.4649(3) -0.34968(11) 0.7870(5) 1.000 0.0442 . . O5 O Uiso 0.3264(5) -0.4594(11) 0.9432(4) 1.000 0.0442 . . O6 O Uiso 0.51439(2) 0.7154(3) 0.2859(3) 1.000 0.0577 . . O7 O Uiso 0.6038(2) -0.00711(3) 0.7238(2) 1.000 0.0577 . . C1 C Uiso 0.08960(19) -0.21208(19) 0.4437(2) 1.000 0.0442 . . C2 C Uiso -0.05027(19) -0.25044(19) 0.47438(19) 1.000 0.0442 . . C3 C Uiso -0.06258(19) -0.33421(17) 0.6165(2) 1.000 0.0442 . . C4 C Uiso 0.06596(19) -0.37852(19) 0.72645(17) 1.000 0.0442 . . C5 C Uiso 0.20346(19) -0.3404(2) 0.6958(19) 1.000 0.0442 . . C6 C Uiso 0.21519(18) -0.25764(17) 0.5555(2) 1.000 0.0442 . . C7 C Uiso -0.0310(2) -0.1068(2) 0.1872(2) 1.000 0.0442 . . C8 C Uiso 0.0023(3) 0.0264(2) 0.0746(2) 1.000 0.0442 . . C9 C Uiso -0.2081(2) -0.3775(3) 0.6544(2) 1.000 0.0442 . . C10 C Uiso 0.3362(2) -0.3872(3) 0.8114(2) 1.000 0.0442 . . H2 H Uiso -0.14189(10) -0.21911(13) 0.39522(13) 1.000 0.0887 . . H4 H Uiso 0.06047(11) -0.43719(15) 0.82772(12) 1.000 0.0887 . . H6 H Uiso 0.31519(11) -0.23094(14) 0.53548(14) 1.000 0.0887 . . H7A H Uiso -0.08433(11) -0.22037(13) 0.1200(12) 1.000 0.0887 . . H7B H Uiso -0.0974(10) -0.0671(13) 0.2465(12) 1.000 0.0887 . . H8 H Uiso 0.01280(12) 0.1537(13) 0.10577(12) 1.000 0.0887 . . #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.973(6) . . yes Zn1 O5 1.864(7) . 1_564 yes Zn1 O1 1.882(8) . 2_556 yes Zn1 O4 1.862(6) . 2_656 yes O1 C9 1.294(4) . . yes O2 C9 1.29(3) . . yes O3 C1 1.430(9) . . yes O3 C7 1.44(2) . . yes O4 C10 1.287(4) . . yes O5 C10 1.289(6) . . yes C1 C2 1.414(3) . . no C1 C6 1.407(2) . . no C2 C3 1.416(2) . . no C3 C4 1.416(2) . . no C3 C9 1.497(3) . . no C4 C5 1.392(6) . . no C5 C6 1.397(13) . . no C5 C10 1.473(10) . . no C7 C8 1.492(2) . . no C8 C8 1.303(3) . 2_555 no C2 H2 1.011(2) . . no C4 H4 0.9976(18) . . no C6 H6 1.003(2) . . no C7 H7A 1.002(6) . . no C7 H7B 1.001(10) . . no C8 H8 1.004(10) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O6 105.2(4) 1_564 . . yes O1 Zn1 O6 111.5(3) 2_556 . . yes O4 Zn1 O6 101.6(3) 2_656 . . yes O1 Zn1 O5 98.6(3) 2_556 . 1_564 yes O4 Zn1 O5 117.2(4) 2_656 . 1_564 yes O1 Zn1 O4 122.1(3) 2_556 . 2_656 yes Zn1 O1 C9 117.9(3) 2_556 . . yes C1 O3 C7 113.3(18) . . . yes Zn1 O4 C10 123.6(2) 2_656 . . yes Zn1 O5 C10 155.5(5) 1_546 . . yes O3 C1 C2 122.1(11) . . . yes O3 C1 C6 118.6(11) . . . yes C2 C1 C6 119.39(15) . . . no C1 C2 C3 119.84(16) . . . no C2 C3 C4 119.36(16) . . . no C2 C3 C9 121.84(16) . . . no C4 C3 C9 118.79(14) . . . no C3 C4 C5 120.6(5) . . . no C4 C5 C6 119.9(7) . . . no C4 C5 C10 120.0(9) . . . no C6 C5 C10 120.2(4) . . . no C1 C6 C5 120.9(3) . . . no O3 C7 C8 108.7(6) . . . yes C7 C8 C8 118.54(14) . . 2_555 no O1 C9 O2 117.9(12) . . . yes O1 C9 C3 119.2(3) . . . yes O2 C9 C3 122.3(11) . . . yes O4 C10 O5 118.9(3) . . . yes O4 C10 C5 120.9(4) . . . yes O5 C10 C5 120.2(5) . . . yes C1 C2 H2 120.53(16) . . . no C3 C2 H2 119.63(18) . . . no C3 C4 H4 120.99(19) . . . no C5 C4 H4 118.4(6) . . . no C1 C6 H6 120.26(16) . . . no C5 C6 H6 118.8(3) . . . no O3 C7 H7A 109.6(4) . . . no O3 C7 H7B 111.3(9) . . . no C8 C7 H7A 109.4(5) . . . no C8 C7 H7B 108.8(6) . . . no H7A C7 H7B 109.1(6) . . . no C7 C8 H8 121.0(3) . . . no C8 C8 H8 119.8(2) 2_555 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zn1 O5 C10 39.8(14) . . 1_564 1_564 no O6 Zn1 O1 C9 -74.9(3) . . 2_556 2_556 no O6 Zn1 O4 C10 -54.3(4) . . 2_656 2_656 no Zn1 O1 C9 O2 9.8(3) 2_556 . . . no Zn1 O1 C9 C3 -178.5(2) 2_556 . . . no C7 O3 C1 C2 -7.0(5) . . . . no C7 O3 C1 C6 173.0(3) . . . . no C1 O3 C7 C8 162.9(3) . . . . no Zn1 O4 C10 O5 38.8(6) 2_656 . . . no Zn1 O4 C10 C5 -144.4(5) 2_656 . . . no Zn1 O5 C10 O4 29.4(15) 1_546 . . . no Zn1 O5 C10 C5 -147.4(12) 1_546 . . . no O3 C1 C2 C3 179.9(2) . . . . no C6 C1 C2 C3 -0.1(2) . . . . no O3 C1 C6 C5 -179.9(4) . . . . no C2 C1 C6 C5 0.2(4) . . . . no C1 C2 C3 C4 0.0(2) . . . . no C1 C2 C3 C9 180.00(17) . . . . no C2 C3 C4 C5 0.0(4) . . . . no C9 C3 C4 C5 -179.9(4) . . . . no C2 C3 C9 O1 -171.21(17) . . . . no C2 C3 C9 O2 0.1(4) . . . . no C4 C3 C9 O1 8.7(3) . . . . no C4 C3 C9 O2 -179.9(3) . . . . no C3 C4 C5 C6 0.0(8) . . . . no C3 C4 C5 C10 180.0(4) . . . . no C4 C5 C6 C1 -0.1(8) . . . . no C10 C5 C6 C1 180.0(4) . . . . no C4 C5 C10 O4 -178.5(4) . . . . no C4 C5 C10 O5 -1.8(9) . . . . no C6 C5 C10 O4 1.4(8) . . . . no C6 C5 C10 O5 178.2(6) . . . . no O3 C7 C8 C8 101.8(5) . . . 2_555 no C7 C8 C8 C7 180.0(2) . . 2_555 2_555 no #END