# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: tubular crystals with controllable channel size and orientation ; loop_ _publ_author_name 'Mir Wais Hosseini' 'Abdelaziz Jouaiti' 'Nathalie Kyritsakas' 'Mei-Jin Lin.' 'Jean-Marc Planeix' ; D.Pocic ; # Attachment 's1339compound1_-_copie.cif' data_e1339a _database_code_depnum_ccdc_archive 'CCDC 743171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 F6 N4 S4 Si Zn, C H Cl3' _chemical_formula_sum 'C25 H25 Cl3 F6 N4 S4 Si Zn' _chemical_formula_weight 823.54 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6873(6) _cell_length_b 7.6211(2) _cell_length_c 24.1630(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.128(3) _cell_angle_gamma 90.00 _cell_volume 3644.78(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4030 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.04 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8886 _exptl_absorpt_correction_T_max 0.9420 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31145 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4174 _reflns_number_gt 3226 _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^)+(0.1245P)^2^+25.7222P] 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 4174 _refine_ls_number_parameters 214 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2214 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.039 _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 Cl3 Cl 0.0442(4) 0.6092(10) 0.0316(3) 0.122(2) Uani 0.50 1 d PD . . C13 C 0.0583(10) 0.821(2) 0.0154(7) 0.106(7) Uiso 0.50 1 d PD . . H13 H 0.0270 0.8965 0.0258 0.127 Uiso 0.50 1 calc PR . . Zn1 Zn 0.0000 0.52597(9) 0.2500 0.0176(2) Uani 1 2 d S . . Si1 Si 0.0000 0.0248(2) 0.2500 0.0184(4) Uani 1 2 d S . . F1 F 0.0000 0.2515(5) 0.2500 0.0265(8) Uani 1 2 d S . . F2 F -0.01940(17) 0.0231(4) 0.30996(14) 0.0325(7) Uani 1 1 d . . . F3 F -0.08162(14) 0.0243(4) 0.20432(15) 0.0343(7) Uani 1 1 d . . . F4 F 0.0000 0.7987(5) 0.2500 0.0257(8) Uani 1 2 d S . . N1 N 0.07962(19) 0.5285(5) 0.21685(17) 0.0206(8) Uani 1 1 d . . . C1 C 0.1163(2) 0.6745(6) 0.2215(2) 0.0256(10) Uani 1 1 d . . . H1 H 0.1033 0.7797 0.2350 0.031 Uiso 1 1 calc R . . C2 C 0.1722(2) 0.6781(6) 0.2075(2) 0.0257(10) Uani 1 1 d . . . H2 H 0.1963 0.7847 0.2108 0.031 Uiso 1 1 calc R . . C3 C 0.1931(2) 0.5261(6) 0.1885(2) 0.0220(9) Uani 1 1 d . . . C4 C 0.1541(2) 0.3757(6) 0.1822(2) 0.0261(10) Uani 1 1 d . . . H4 H 0.1655 0.2691 0.1681 0.031 Uiso 1 1 calc R . . C5 C 0.0983(2) 0.3842(6) 0.1968(2) 0.0261(10) Uani 1 1 d . . . H5 H 0.0720 0.2810 0.1921 0.031 Uiso 1 1 calc R . . S1 S 0.26785(6) 0.53903(16) 0.17778(5) 0.0257(3) Uani 1 1 d . . . C6 C 0.2692(2) 0.3381(6) 0.1394(2) 0.0251(9) Uani 1 1 d . . . H6A H 0.3148 0.3232 0.1398 0.030 Uiso 1 1 calc R . . H6B H 0.2615 0.2391 0.1623 0.030 Uiso 1 1 calc R . . C7 C 0.2171(2) 0.3280(7) 0.0739(2) 0.0262(10) Uani 1 1 d . . . H7A H 0.1718 0.3592 0.0717 0.031 Uiso 1 1 calc R . . H7B H 0.2151 0.2071 0.0582 0.031 Uiso 1 1 calc R . . S2 S 0.24153(6) 0.47905(17) 0.02906(5) 0.0281(3) Uani 1 1 d . . . C8 C 0.1752(2) 0.4676(6) -0.0431(2) 0.0228(9) Uani 1 1 d . . . C9 C 0.1224(2) 0.3475(6) -0.0609(2) 0.0244(9) Uani 1 1 d . . . H9 H 0.1195 0.2628 -0.0332 0.029 Uiso 1 1 calc R . . C10 C 0.0743(2) 0.3544(6) -0.1198(2) 0.0250(9) Uani 1 1 d . . . H10 H 0.0386 0.2711 -0.1320 0.030 Uiso 1 1 calc R . . N2 N 0.07506(19) 0.4715(5) -0.16063(17) 0.0208(8) Uani 1 1 d . . . C11 C 0.1261(2) 0.5862(6) -0.1433(2) 0.0264(10) Uani 1 1 d . . . H11 H 0.1273 0.6699 -0.1720 0.032 Uiso 1 1 calc R . . C12 C 0.1769(2) 0.5885(7) -0.0859(2) 0.0287(10) Uani 1 1 d . . . H12 H 0.2127 0.6712 -0.0755 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.0436(3) 0.8688(9) -0.0588(2) 0.1050(19) Uani 0.50 1 d PD . . Cl2 Cl 0.1341(5) 0.8883(15) 0.0568(5) 0.181(4) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl3 0.115(5) 0.140(6) 0.135(5) 0.033(5) 0.077(4) 0.028(4) Zn1 0.0168(4) 0.0161(4) 0.0199(4) 0.000 0.0076(3) 0.000 Si1 0.0158(8) 0.0139(8) 0.0261(9) 0.000 0.0092(7) 0.000 F1 0.0296(19) 0.0158(17) 0.039(2) 0.000 0.0190(17) 0.000 F2 0.0487(19) 0.0222(14) 0.0380(17) 0.0014(12) 0.0294(15) 0.0032(12) F3 0.0200(14) 0.0284(15) 0.0457(19) 0.0027(13) 0.0044(13) -0.0005(11) F4 0.0288(19) 0.0136(17) 0.039(2) 0.000 0.0181(17) 0.000 N1 0.0179(17) 0.0214(19) 0.0222(19) -0.0010(14) 0.0077(14) 0.0006(14) C1 0.025(2) 0.019(2) 0.035(3) -0.0042(19) 0.0141(19) -0.0022(18) C2 0.024(2) 0.023(2) 0.033(2) -0.0016(19) 0.0147(19) -0.0039(18) C3 0.019(2) 0.030(2) 0.017(2) -0.0040(17) 0.0074(17) -0.0019(17) C4 0.030(2) 0.023(2) 0.035(3) -0.0047(19) 0.023(2) -0.0031(18) C5 0.028(2) 0.025(2) 0.031(2) -0.0021(19) 0.017(2) -0.0017(18) S1 0.0215(6) 0.0324(7) 0.0267(6) -0.0060(5) 0.0134(5) -0.0036(4) C6 0.022(2) 0.032(2) 0.022(2) -0.0005(18) 0.0091(17) 0.0056(18) C7 0.025(2) 0.030(2) 0.022(2) 0.0004(18) 0.0073(18) 0.0003(19) S2 0.0262(6) 0.0335(7) 0.0197(6) -0.0012(5) 0.0043(5) -0.0057(5) C8 0.021(2) 0.024(2) 0.022(2) -0.0030(17) 0.0077(18) 0.0012(17) C9 0.028(2) 0.024(2) 0.021(2) 0.0047(17) 0.0104(18) 0.0007(18) C10 0.021(2) 0.027(2) 0.025(2) 0.0014(18) 0.0073(18) -0.0039(17) N2 0.0200(17) 0.0210(18) 0.0204(18) -0.0013(14) 0.0071(14) 0.0000(14) C11 0.028(2) 0.023(2) 0.025(2) 0.0035(18) 0.0071(19) -0.0015(19) C12 0.026(2) 0.028(2) 0.028(2) -0.002(2) 0.0062(19) -0.0067(19) Cl1 0.139(5) 0.134(5) 0.057(3) -0.015(3) 0.055(3) -0.016(4) Cl2 0.179(9) 0.194(10) 0.200(10) 0.082(8) 0.107(8) 0.000(7) _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 Cl3 C13 1.715(15) . ? C13 Cl2 1.621(16) . ? C13 Cl1 1.726(15) . ? C13 H13 1.0000 . ? Zn1 F4 2.078(4) . ? Zn1 F1 2.092(4) . ? Zn1 N2 2.107(4) 6_566 ? Zn1 N2 2.107(4) 5_565 ? Zn1 N1 2.180(4) 2 ? Zn1 N1 2.180(4) . ? Si1 F3 1.660(3) 2 ? Si1 F3 1.660(3) . ? Si1 F2 1.666(3) . ? Si1 F2 1.666(3) 2 ? Si1 F4 1.723(4) 1_545 ? Si1 F1 1.728(4) . ? F4 Si1 1.723(4) 1_565 ? N1 C5 1.330(6) . ? N1 C1 1.345(6) . ? C1 C2 1.388(7) . ? C1 H1 0.9500 . ? C2 C3 1.389(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(6) . ? C3 S1 1.745(5) . ? C4 C5 1.396(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? S1 C6 1.797(5) . ? C6 C7 1.525(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 S2 1.803(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? S2 C8 1.751(5) . ? C8 C9 1.390(6) . ? C8 C12 1.397(7) . ? C9 C10 1.379(6) . ? C9 H9 0.9500 . ? C10 N2 1.336(6) . ? C10 H10 0.9500 . ? N2 C11 1.336(6) . ? N2 Zn1 2.107(4) 5_565 ? C11 C12 1.375(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? 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 Cl2 C13 Cl3 112.9(11) . . ? Cl2 C13 Cl1 106.5(11) . . ? Cl3 C13 Cl1 117.6(11) . . ? Cl2 C13 H13 106.4 . . ? Cl3 C13 H13 106.4 . . ? Cl1 C13 H13 106.4 . . ? F4 Zn1 F1 180.000(1) . . ? F4 Zn1 N2 89.47(10) . 6_566 ? F1 Zn1 N2 90.53(10) . 6_566 ? F4 Zn1 N2 89.47(10) . 5_565 ? F1 Zn1 N2 90.53(10) . 5_565 ? N2 Zn1 N2 178.9(2) 6_566 5_565 ? F4 Zn1 N1 89.49(10) . 2 ? F1 Zn1 N1 90.51(10) . 2 ? N2 Zn1 N1 91.12(14) 6_566 2 ? N2 Zn1 N1 88.87(14) 5_565 2 ? F4 Zn1 N1 89.49(10) . . ? F1 Zn1 N1 90.51(10) . . ? N2 Zn1 N1 88.87(14) 6_566 . ? N2 Zn1 N1 91.12(14) 5_565 . ? N1 Zn1 N1 178.98(19) 2 . ? F3 Si1 F3 179.7(2) 2 . ? F3 Si1 F2 90.08(17) 2 . ? F3 Si1 F2 89.92(17) . . ? F3 Si1 F2 89.92(17) 2 2 ? F3 Si1 F2 90.08(17) . 2 ? F2 Si1 F2 179.1(2) . 2 ? F3 Si1 F4 89.87(11) 2 1_545 ? F3 Si1 F4 89.87(11) . 1_545 ? F2 Si1 F4 89.55(11) . 1_545 ? F2 Si1 F4 89.54(11) 2 1_545 ? F3 Si1 F1 90.13(11) 2 . ? F3 Si1 F1 90.13(11) . . ? F2 Si1 F1 90.46(11) . . ? F2 Si1 F1 90.46(11) 2 . ? F4 Si1 F1 179.999(1) 1_545 . ? Si1 F1 Zn1 180.0 . . ? Si1 F4 Zn1 180.0 1_565 . ? C5 N1 C1 117.2(4) . . ? C5 N1 Zn1 122.1(3) . . ? C1 N1 Zn1 120.4(3) . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 120.0(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 117.2(4) . . ? C2 C3 S1 116.7(3) . . ? C4 C3 S1 126.0(4) . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 123.8(4) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C3 S1 C6 103.9(2) . . ? C7 C6 S1 114.7(3) . . ? C7 C6 H6A 108.6 . . ? S1 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? S1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C6 C7 S2 108.4(3) . . ? C6 C7 H7A 110.0 . . ? S2 C7 H7A 110.0 . . ? C6 C7 H7B 110.0 . . ? S2 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C8 S2 C7 104.1(2) . . ? C9 C8 C12 118.3(4) . . ? C9 C8 S2 125.3(4) . . ? C12 C8 S2 116.4(3) . . ? C10 C9 C8 118.3(4) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N2 C10 C9 123.7(4) . . ? N2 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C10 N2 C11 117.7(4) . . ? C10 N2 Zn1 121.7(3) . 5_565 ? C11 N2 Zn1 120.6(3) . 5_565 ? N2 C11 C12 123.0(5) . . ? N2 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C8 119.0(4) . . ? C11 C12 H12 120.5 . . ? C8 C12 H12 120.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.340 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.146 # Attachment 's1540compound3_-_copie.cif' data_e1540a _database_code_depnum_ccdc_archive 'CCDC 743172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 F6 N4 S4 Si Zn' _chemical_formula_sum 'C28 H32 F6 N4 S4 Si Zn' _chemical_formula_weight 760.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6498(14) _cell_length_b 7.7080(5) _cell_length_c 28.670(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.5450(10) _cell_angle_gamma 90.00 _cell_volume 4450.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4086 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas colorless _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9454 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12211 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4889 _reflns_number_gt 3809 _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^)+(0.1091P)^2^+20.8235P] 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 4889 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.33949(7) 0.2500 0.01571(19) Uani 1 2 d S . . Si1 Si 0.5000 0.83842(17) 0.2500 0.0176(3) Uani 1 2 d S . . F1 F 0.5000 0.0621(4) 0.2500 0.0218(7) Uani 1 2 d S . . F2 F 0.5000 0.6144(4) 0.2500 0.0258(7) Uani 1 2 d S . . F3 F 0.42554(12) 0.8410(3) 0.20303(10) 0.0317(6) Uani 1 1 d . . . F4 F 0.53669(14) 0.8388(3) 0.20837(11) 0.0335(6) Uani 1 1 d . . . N1 N 0.39339(15) 0.3387(4) 0.22786(12) 0.0189(6) Uani 1 1 d . . . C1 C 0.3606(2) 0.1953(5) 0.23171(16) 0.0238(8) Uani 1 1 d . . . H1 H 0.3853 0.0917 0.2434 0.029 Uiso 1 1 calc R . . C2 C 0.29310(19) 0.1913(5) 0.21949(16) 0.0233(8) Uani 1 1 d . . . H2 H 0.2722 0.0862 0.2229 0.028 Uiso 1 1 calc R . . C3 C 0.25480(18) 0.3410(5) 0.20210(14) 0.0208(8) Uani 1 1 d . . . C4 C 0.28911(19) 0.4890(5) 0.19747(16) 0.0264(9) Uani 1 1 d . . . H4 H 0.2657 0.5940 0.1853 0.032 Uiso 1 1 calc R . . C5 C 0.3567(2) 0.4826(5) 0.21048(16) 0.0264(9) Uani 1 1 d . . . H5 H 0.3789 0.5854 0.2071 0.032 Uiso 1 1 calc R . . S1 S 0.17031(5) 0.32674(14) 0.19174(4) 0.0266(3) Uani 1 1 d . . . C6 C 0.1355(2) 0.5220(6) 0.15651(16) 0.0297(9) Uani 1 1 d . . . H6A H 0.0903 0.5394 0.1566 0.036 Uiso 1 1 calc R . . H6B H 0.1629 0.6224 0.1739 0.036 Uiso 1 1 calc R . . C7 C 0.1316(2) 0.5202(7) 0.10234(18) 0.0361(10) Uani 1 1 d . . . H7A H 0.1160 0.6348 0.0869 0.043 Uiso 1 1 calc R . . H7B H 0.1765 0.5001 0.1018 0.043 Uiso 1 1 calc R . . C8 C 0.0850(3) 0.3809(7) 0.07183(19) 0.0420(12) Uani 1 1 d . . . H8A H 0.0403 0.4002 0.0729 0.050 Uiso 1 1 calc R . . H8B H 0.1010 0.2663 0.0871 0.050 Uiso 1 1 calc R . . C9 C 0.4202(3) 0.1209(7) -0.01721(19) 0.0435(12) Uani 1 1 d . . . H9A H 0.4371 0.0084 -0.0009 0.052 Uiso 1 1 calc R . . H9B H 0.3762 0.1432 -0.0152 0.052 Uiso 1 1 calc R . . S2 S 0.47722(8) 0.2932(2) 0.01262(5) 0.0491(4) Uani 1 1 d . . . C10 C 0.4804(3) 0.2988(6) 0.07457(17) 0.0338(10) Uani 1 1 d . . . C11 C 0.5170(3) 0.4302(7) 0.10460(19) 0.0454(13) Uani 1 1 d . . . H11 H 0.5393 0.5125 0.0917 0.054 Uiso 1 1 calc R . . C12 C 0.5209(3) 0.4410(6) 0.15377(17) 0.0333(10) Uani 1 1 d . . . H12 H 0.5459 0.5329 0.1741 0.040 Uiso 1 1 calc R . . N2 N 0.49077(16) 0.3271(4) 0.17408(13) 0.0222(7) Uani 1 1 d . . . C13 C 0.4554(2) 0.1992(5) 0.14427(15) 0.0251(8) Uani 1 1 d . . . H13 H 0.4340 0.1171 0.1580 0.030 Uiso 1 1 calc R . . C14 C 0.4487(2) 0.1817(6) 0.09522(17) 0.0308(9) Uani 1 1 d . . . H14 H 0.4226 0.0904 0.0754 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0146(3) 0.0134(3) 0.0197(3) 0.000 0.0070(2) 0.000 Si1 0.0159(6) 0.0104(6) 0.0275(8) 0.000 0.0093(6) 0.000 F1 0.0239(15) 0.0063(13) 0.0347(18) 0.000 0.0100(14) 0.000 F2 0.0230(16) 0.0135(15) 0.0380(19) 0.000 0.0076(14) 0.000 F3 0.0246(12) 0.0200(12) 0.0421(15) 0.0014(10) 0.0022(11) -0.0022(9) F4 0.0410(15) 0.0245(13) 0.0451(16) -0.0021(11) 0.0276(13) -0.0020(10) N1 0.0167(14) 0.0185(16) 0.0218(16) 0.0012(12) 0.0076(13) 0.0008(11) C1 0.0218(18) 0.0207(19) 0.030(2) 0.0039(15) 0.0102(17) 0.0010(14) C2 0.0199(18) 0.0199(18) 0.032(2) 0.0027(15) 0.0115(16) -0.0018(14) C3 0.0173(16) 0.025(2) 0.0197(18) -0.0010(15) 0.0069(15) -0.0026(14) C4 0.0207(18) 0.023(2) 0.033(2) 0.0041(17) 0.0066(16) 0.0032(15) C5 0.0218(18) 0.022(2) 0.033(2) 0.0032(16) 0.0077(17) -0.0010(15) S1 0.0157(4) 0.0344(6) 0.0289(5) 0.0014(4) 0.0072(4) -0.0009(4) C6 0.0239(19) 0.038(2) 0.023(2) 0.0027(18) 0.0040(16) 0.0095(17) C7 0.033(2) 0.041(3) 0.033(2) 0.002(2) 0.0107(19) 0.000(2) C8 0.047(3) 0.048(3) 0.032(3) -0.001(2) 0.016(2) -0.008(2) C9 0.050(3) 0.048(3) 0.030(2) -0.006(2) 0.011(2) -0.010(2) S2 0.0715(10) 0.0522(8) 0.0257(6) -0.0043(5) 0.0205(6) -0.0200(7) C10 0.042(3) 0.040(2) 0.021(2) -0.0010(18) 0.0132(19) -0.008(2) C11 0.069(4) 0.039(3) 0.032(3) -0.002(2) 0.024(3) -0.022(3) C12 0.046(3) 0.030(2) 0.026(2) -0.0055(18) 0.016(2) -0.0135(19) N2 0.0197(15) 0.0227(17) 0.0235(17) -0.0025(13) 0.0071(13) -0.0035(12) C13 0.0257(19) 0.026(2) 0.022(2) -0.0027(16) 0.0073(16) -0.0050(15) C14 0.034(2) 0.033(2) 0.026(2) -0.0040(17) 0.0106(18) -0.0066(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 N2 2.114(4) . ? Zn1 N2 2.114(4) 2_655 ? Zn1 F2 2.119(3) . ? Zn1 F1 2.138(3) . ? Zn1 N1 2.157(3) 2_655 ? Zn1 N1 2.157(3) . ? Si1 F4 1.659(3) . ? Si1 F4 1.659(3) 2_655 ? Si1 F3 1.679(2) 2_655 ? Si1 F3 1.679(2) . ? Si1 F1 1.724(3) 1_565 ? Si1 F2 1.727(3) . ? F1 Si1 1.724(3) 1_545 ? N1 C1 1.340(5) . ? N1 C5 1.349(5) . ? C1 C2 1.373(5) . ? C1 H1 0.9500 . ? C2 C3 1.402(5) . ? C2 H2 0.9500 . ? C3 C4 1.393(6) . ? C3 S1 1.746(4) . ? C4 C5 1.372(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? S1 C6 1.815(4) . ? C6 C7 1.524(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.512(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.528(7) 7 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C8 1.528(7) 7 ? C9 S2 1.801(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? S2 C10 1.752(5) . ? C10 C11 1.376(7) . ? C10 C14 1.391(6) . ? C11 C12 1.383(7) . ? C11 H11 0.9500 . ? C12 N2 1.346(6) . ? C12 H12 0.9500 . ? N2 C13 1.345(5) . ? C13 C14 1.366(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? 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 N2 Zn1 N2 174.81(18) . 2_655 ? N2 Zn1 F2 92.59(9) . . ? N2 Zn1 F2 92.59(9) 2_655 . ? N2 Zn1 F1 87.41(9) . . ? N2 Zn1 F1 87.41(9) 2_655 . ? F2 Zn1 F1 180.000(1) . . ? N2 Zn1 N1 89.39(13) . 2_655 ? N2 Zn1 N1 90.60(13) 2_655 2_655 ? F2 Zn1 N1 90.16(8) . 2_655 ? F1 Zn1 N1 89.84(8) . 2_655 ? N2 Zn1 N1 90.60(13) . . ? N2 Zn1 N1 89.38(13) 2_655 . ? F2 Zn1 N1 90.16(8) . . ? F1 Zn1 N1 89.84(8) . . ? N1 Zn1 N1 179.67(16) 2_655 . ? F4 Si1 F4 179.78(19) . 2_655 ? F4 Si1 F3 90.26(14) . 2_655 ? F4 Si1 F3 89.74(14) 2_655 2_655 ? F4 Si1 F3 89.74(14) . . ? F4 Si1 F3 90.26(14) 2_655 . ? F3 Si1 F3 178.67(18) 2_655 . ? F4 Si1 F1 89.90(9) . 1_565 ? F4 Si1 F1 89.89(9) 2_655 1_565 ? F3 Si1 F1 89.33(9) 2_655 1_565 ? F3 Si1 F1 89.33(9) . 1_565 ? F4 Si1 F2 90.11(9) . . ? F4 Si1 F2 90.11(9) 2_655 . ? F3 Si1 F2 90.67(9) 2_655 . ? F3 Si1 F2 90.67(9) . . ? F1 Si1 F2 179.996(2) 1_565 . ? Si1 F1 Zn1 179.996(1) 1_545 . ? Si1 F2 Zn1 180.0 . . ? C1 N1 C5 116.9(3) . . ? C1 N1 Zn1 121.3(3) . . ? C5 N1 Zn1 121.8(3) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 120.5(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 116.2(3) . . ? C4 C3 S1 126.7(3) . . ? C2 C3 S1 117.0(3) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.6(4) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C3 S1 C6 103.7(2) . . ? C7 C6 S1 114.6(3) . . ? C7 C6 H6A 108.6 . . ? S1 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? S1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C6 111.8(4) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 112.4(4) . 7 ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 7 . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 7 . ? H8A C8 H8B 107.9 . . ? C8 C9 S2 105.8(4) 7 . ? C8 C9 H9A 110.6 7 . ? S2 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 7 . ? S2 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C10 S2 C9 105.3(2) . . ? C11 C10 C14 118.1(4) . . ? C11 C10 S2 116.9(4) . . ? C14 C10 S2 125.0(4) . . ? C10 C11 C12 119.2(4) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N2 C12 C11 122.9(4) . . ? N2 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C13 N2 C12 117.2(4) . . ? C13 N2 Zn1 120.3(3) . . ? C12 N2 Zn1 122.6(3) . . ? N2 C13 C14 123.1(4) . . ? N2 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.5(4) . . ? C13 C14 H14 120.3 . . ? C10 C14 H14 120.3 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.217 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.195 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 -0.105 0.000 448.3 144.7 2 0.750 0.049 0.000 448.3 144.7 3 0.750 -0.112 0.500 448.4 144.0 4 0.250 0.049 0.500 448.4 144.0 _platon_squeeze_details ; ; # Attachment 'New Cif compound4.cif' data_e1286a _database_code_depnum_ccdc_archive 'CCDC 743173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 F6 N4 O4 S4 Si Zn, 2(C2 H6 O), 0.25(C4 H4 Cl12)' _chemical_formula_sum 'C30.50 H30.50 Cl1.50 F6 N4 O5 S4 Si Zn' _chemical_formula_weight 921.96 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.512(2) _cell_length_b 14.5274(17) _cell_length_c 15.2352(16) _cell_angle_alpha 90.00 _cell_angle_beta 112.227(3) _cell_angle_gamma 90.00 _cell_volume 4612.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1095 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.39 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8784 _exptl_absorpt_correction_T_max 0.9165 _exptl_absorpt_process_details sadabs _exptl_special_details ; There is a disorder with the chloroform and ethanol molecules. The chloroform has a 25% occupancy and the ethanol has a 50 % occupancy according to the B of the structure ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15152 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5237 _reflns_number_gt 4160 _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5237 _refine_ls_number_parameters 280 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.1157 _refine_ls_wR_factor_ref 0.3703 _refine_ls_wR_factor_gt 0.3446 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.0000 0.0000 0.0200(4) Uani 1 2 d S . . Si1 Si 0.5000 0.01518(16) 0.2500 0.0189(5) Uani 1 2 d S . . F1 F 0.49825(18) 0.0142(3) 0.1351(3) 0.0256(9) Uani 1 1 d . . . F2 F 0.5000 0.1292(4) 0.2500 0.0376(14) Uani 1 2 d S . . F3 F 0.42040(19) 0.0140(3) 0.2077(3) 0.0327(10) Uani 1 1 d . . . F4 F 0.5000 -0.1003(4) 0.2500 0.0316(12) Uani 1 2 d S . . N1 N 0.5801(3) -0.0948(4) 0.0507(4) 0.0259(11) Uani 1 1 d . . . C1 C 0.6176(4) -0.1182(6) 0.0052(5) 0.0377(17) Uani 1 1 d . . . H1 H 0.6099 -0.0897 -0.0542 0.045 Uiso 1 1 calc R . . C2 C 0.6673(4) -0.1815(6) 0.0383(6) 0.0395(18) Uani 1 1 d . . . H2 H 0.6936 -0.1946 0.0036 0.047 Uiso 1 1 calc R . . C3 C 0.6773(3) -0.2251(5) 0.1236(5) 0.0277(13) Uani 1 1 d . . . C4 C 0.6387(3) -0.2027(5) 0.1723(5) 0.0312(14) Uani 1 1 d . . . H4 H 0.6447 -0.2318 0.2309 0.037 Uiso 1 1 calc R . . C5 C 0.5910(3) -0.1375(5) 0.1349(5) 0.0301(14) Uani 1 1 d . . . H5 H 0.5650 -0.1219 0.1693 0.036 Uiso 1 1 calc R . . C6 C 0.7298(3) -0.2970(5) 0.1583(5) 0.0325(15) Uani 1 1 d . . . O1 O 0.7694(3) -0.3052(4) 0.1249(4) 0.0482(15) Uani 1 1 d . . . S1 S 0.72605(9) -0.36795(13) 0.24984(13) 0.0348(5) Uani 1 1 d . . . C7 C 0.7888(4) -0.4470(5) 0.2575(5) 0.0372(16) Uani 1 1 d . . . H7A H 0.8261 -0.4117 0.2565 0.045 Uiso 1 1 calc R . . H7B H 0.8023 -0.4796 0.3190 0.045 Uiso 1 1 calc R . . C8 C 0.7700(4) 0.4822(5) 0.1784(6) 0.0357(16) Uani 1 1 d . . . H8A H 0.8081 0.4452 0.1833 0.043 Uiso 1 1 calc R . . H8B H 0.7544 0.5139 0.1163 0.043 Uiso 1 1 calc R . . S2 S 0.70796(10) 0.40694(15) 0.18543(15) 0.0428(6) Uani 1 1 d . . . C9 C 0.6959(4) 0.3403(5) 0.0848(6) 0.0392(17) Uani 1 1 d . . . O2 O 0.7235(3) 0.3560(5) 0.0304(6) 0.062(2) Uani 1 1 d . . . C10 C 0.6481(3) 0.2632(5) 0.0664(5) 0.0312(14) Uani 1 1 d . . . C11 C 0.6458(4) 0.1989(6) -0.0017(6) 0.0384(17) Uani 1 1 d . . . H11 H 0.6735 0.2044 -0.0354 0.046 Uiso 1 1 calc R . . C12 C 0.6025(3) 0.1262(5) -0.0203(5) 0.0333(15) Uani 1 1 d . . . H12 H 0.6005 0.0828 -0.0681 0.040 Uiso 1 1 calc R . . N2 N 0.5634(3) 0.1155(4) 0.0276(4) 0.0247(11) Uani 1 1 d . . . C13 C 0.5655(3) 0.1791(5) 0.0929(5) 0.0306(14) Uani 1 1 d . . . H13 H 0.5374 0.1724 0.1258 0.037 Uiso 1 1 calc R . . C14 C 0.6065(4) 0.2530(5) 0.1143(5) 0.0350(15) Uani 1 1 d . . . H14 H 0.6065 0.2966 0.1608 0.042 Uiso 1 1 calc R . . C15 C 0.5883(14) 0.592(2) 0.8924(17) 0.0384(17) Uani 0.25 1 d P . . H15 H 0.5637 0.5433 0.8460 0.046 Uiso 0.25 1 calc PR . . Cl1 Cl 0.6798(6) 0.5779(7) 0.9176(6) 0.067(3) Uani 0.25 1 d P . . Cl2 Cl 0.5675(4) 0.7006(5) 0.8400(5) 0.0448(18) Uani 0.25 1 d P . . Cl3 Cl 0.5899(7) 0.5655(10) 0.9966(6) 0.099(6) Uani 0.25 1 d P . . O3 O 0.5817(5) 0.3599(7) 0.8066(10) 0.0384(17) Uani 0.50 1 d PD F -1 H3 H 0.5839 0.4148 0.8248 0.046 Uiso 0.50 1 calc PR F -1 C16 C 0.5233(13) 0.316(2) 0.812(2) 0.106(10) Uiso 0.50 1 d PD F -1 H16A H 0.5343 0.2509 0.8312 0.128 Uiso 0.50 1 calc PR F -1 H16B H 0.4902 0.3146 0.7467 0.128 Uiso 0.50 1 calc PR F -1 C17 C 0.4919(6) 0.3572(8) 0.8777(9) 0.025(3) Uani 0.50 1 d PD F -1 H17A H 0.5207 0.4032 0.9194 0.038 Uiso 0.50 1 calc PR F -1 H17B H 0.4841 0.3081 0.9161 0.038 Uiso 0.50 1 calc PR F -1 H17C H 0.4511 0.3864 0.8391 0.038 Uiso 0.50 1 calc PR F -1 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 0.0209(6) 0.0248(6) 0.0160(6) 0.0006(3) 0.0088(4) 0.0000(3) Si1 0.0208(11) 0.0232(11) 0.0140(11) 0.000 0.0079(9) 0.000 F1 0.027(2) 0.034(2) 0.0182(17) 0.0011(14) 0.0107(15) 0.0021(14) F2 0.064(4) 0.021(3) 0.037(3) 0.000 0.030(3) 0.000 F3 0.0198(19) 0.058(3) 0.0215(19) 0.0002(17) 0.0091(15) 0.0019(16) F4 0.048(3) 0.025(3) 0.033(3) 0.000 0.028(3) 0.000 N1 0.025(3) 0.029(3) 0.023(2) 0.002(2) 0.007(2) 0.001(2) C1 0.040(4) 0.049(4) 0.029(3) 0.012(3) 0.018(3) 0.011(3) C2 0.034(4) 0.055(5) 0.035(4) 0.012(3) 0.020(3) 0.013(3) C3 0.028(3) 0.028(3) 0.028(3) 0.007(2) 0.012(3) 0.004(2) C4 0.043(4) 0.031(3) 0.023(3) 0.008(2) 0.016(3) 0.010(3) C5 0.034(3) 0.038(4) 0.024(3) 0.000(3) 0.017(3) 0.011(3) C6 0.033(3) 0.034(4) 0.034(3) 0.005(3) 0.017(3) 0.007(3) O1 0.048(3) 0.054(4) 0.054(3) 0.015(3) 0.032(3) 0.024(3) S1 0.0351(10) 0.0327(10) 0.0373(10) 0.0073(7) 0.0145(8) 0.0075(7) C7 0.034(4) 0.032(4) 0.038(4) -0.002(3) 0.006(3) 0.002(3) C8 0.037(4) 0.025(3) 0.044(4) -0.003(3) 0.015(3) -0.003(3) S2 0.0428(11) 0.0428(11) 0.0435(11) -0.0071(8) 0.0172(9) -0.0167(8) C9 0.033(4) 0.034(4) 0.054(5) -0.008(3) 0.020(3) -0.006(3) O2 0.066(4) 0.060(4) 0.081(5) -0.029(4) 0.053(4) -0.034(3) C10 0.023(3) 0.032(3) 0.038(3) 0.001(3) 0.011(3) -0.004(2) C11 0.034(4) 0.048(4) 0.042(4) -0.012(3) 0.026(3) -0.012(3) C12 0.032(3) 0.040(4) 0.032(3) -0.011(3) 0.016(3) -0.007(3) N2 0.023(2) 0.029(3) 0.023(2) 0.002(2) 0.010(2) 0.000(2) C13 0.031(3) 0.033(4) 0.035(3) 0.001(3) 0.020(3) -0.004(3) C14 0.038(4) 0.031(3) 0.042(4) -0.009(3) 0.023(3) -0.005(3) C15 0.034(4) 0.048(4) 0.042(4) -0.012(3) 0.026(3) -0.012(3) Cl1 0.104(8) 0.041(5) 0.033(4) 0.007(3) 0.000(4) 0.007(5) Cl2 0.065(5) 0.030(3) 0.026(3) 0.006(3) 0.001(3) 0.000(3) Cl3 0.148(12) 0.119(10) 0.027(4) 0.003(5) 0.029(5) -0.093(10) O3 0.034(4) 0.048(4) 0.042(4) -0.012(3) 0.026(3) -0.012(3) C17 0.019(5) 0.021(6) 0.037(7) -0.016(5) 0.013(5) -0.019(4) _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 F1 2.084(4) 5_655 ? Zn1 F1 2.084(4) . ? Zn1 N2 2.138(5) . ? Zn1 N2 2.138(5) 5_655 ? Zn1 N1 2.166(6) . ? Zn1 N1 2.166(6) 5_655 ? Si1 F2 1.657(6) . ? Si1 F3 1.659(4) 2_655 ? Si1 F3 1.659(4) . ? Si1 F4 1.678(6) . ? Si1 F1 1.736(4) . ? Si1 F1 1.736(4) 2_655 ? N1 C1 1.323(9) . ? N1 C5 1.361(9) . ? C1 C2 1.388(10) . ? C1 H1 0.9500 . ? C2 C3 1.386(10) . ? C2 H2 0.9500 . ? C3 C4 1.378(9) . ? C3 C6 1.515(9) . ? C4 C5 1.381(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O1 1.188(9) . ? C6 S1 1.762(7) . ? S1 C7 1.789(8) . ? C7 C8 1.518(10) 1_545 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C7 1.518(10) 1_565 ? C8 S2 1.809(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? S2 C9 1.746(8) . ? C9 O2 1.230(10) . ? C9 C10 1.505(10) . ? C10 C11 1.382(10) . ? C10 C14 1.394(10) . ? C11 C12 1.392(10) . ? C11 H11 0.9500 . ? C12 N2 1.350(9) . ? C12 H12 0.9500 . ? N2 C13 1.344(9) . ? C13 C14 1.372(10) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 Cl3 1.62(3) . ? C15 Cl2 1.76(3) . ? C15 Cl1 1.96(3) . ? C15 H15 1.0000 . ? O3 C16 1.492(17) . ? O3 H3 0.8400 . ? C16 C17 1.551(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 F1 Zn1 F1 180.0 5_655 . ? F1 Zn1 N2 90.67(17) 5_655 . ? F1 Zn1 N2 89.34(17) . . ? F1 Zn1 N2 89.33(17) 5_655 5_655 ? F1 Zn1 N2 90.66(17) . 5_655 ? N2 Zn1 N2 180.0 . 5_655 ? F1 Zn1 N1 88.01(17) 5_655 . ? F1 Zn1 N1 91.99(17) . . ? N2 Zn1 N1 91.5(2) . . ? N2 Zn1 N1 88.5(2) 5_655 . ? F1 Zn1 N1 91.99(17) 5_655 5_655 ? F1 Zn1 N1 88.01(17) . 5_655 ? N2 Zn1 N1 88.5(2) . 5_655 ? N2 Zn1 N1 91.5(2) 5_655 5_655 ? N1 Zn1 N1 179.997(1) . 5_655 ? F2 Si1 F3 90.60(18) . 2_655 ? F2 Si1 F3 90.59(18) . . ? F3 Si1 F3 178.8(4) 2_655 . ? F2 Si1 F4 180.000(1) . . ? F3 Si1 F4 89.40(18) 2_655 . ? F3 Si1 F4 89.41(18) . . ? F2 Si1 F1 90.47(15) . . ? F3 Si1 F1 90.03(18) 2_655 . ? F3 Si1 F1 89.96(18) . . ? F4 Si1 F1 89.53(15) . . ? F2 Si1 F1 90.47(15) . 2_655 ? F3 Si1 F1 89.96(18) 2_655 2_655 ? F3 Si1 F1 90.03(18) . 2_655 ? F4 Si1 F1 89.53(15) . 2_655 ? F1 Si1 F1 179.1(3) . 2_655 ? Si1 F1 Zn1 174.3(2) . . ? C1 N1 C5 117.0(6) . . ? C1 N1 Zn1 125.9(5) . . ? C5 N1 Zn1 117.1(4) . . ? N1 C1 C2 124.4(7) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 117.8(7) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 119.0(6) . . ? C4 C3 C6 123.0(6) . . ? C2 C3 C6 118.1(6) . . ? C3 C4 C5 119.4(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 122.4(6) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? O1 C6 C3 122.2(6) . . ? O1 C6 S1 123.3(6) . . ? C3 C6 S1 114.4(5) . . ? C6 S1 C7 98.8(4) . . ? C8 C7 S1 114.1(5) 1_545 . ? C8 C7 H7A 108.7 1_545 . ? S1 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 1_545 . ? S1 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 S2 110.6(6) 1_565 . ? C7 C8 H8A 109.5 1_565 . ? S2 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 1_565 . ? S2 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C9 S2 C8 98.6(4) . . ? O2 C9 C10 121.4(7) . . ? O2 C9 S2 122.6(6) . . ? C10 C9 S2 116.0(5) . . ? C11 C10 C14 118.6(6) . . ? C11 C10 C9 117.6(6) . . ? C14 C10 C9 123.8(7) . . ? C10 C11 C12 119.4(6) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N2 C12 C11 121.7(6) . . ? N2 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C13 N2 C12 118.2(6) . . ? C13 N2 Zn1 121.3(4) . . ? C12 N2 Zn1 120.5(5) . . ? N2 C13 C14 123.1(6) . . ? N2 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 118.8(6) . . ? C13 C14 H14 120.6 . . ? C10 C14 H14 120.6 . . ? Cl3 C15 Cl2 124(2) . . ? Cl3 C15 Cl1 98.8(13) . . ? Cl2 C15 Cl1 105.1(16) . . ? Cl3 C15 H15 109.2 . . ? Cl2 C15 H15 109.2 . . ? Cl1 C15 H15 109.2 . . ? O3 C16 C17 119.6(16) . . ? O3 C16 H16A 107.4 . . ? C17 C16 H16A 107.4 . . ? O3 C16 H16B 107.4 . . ? C17 C16 H16B 107.4 . . ? H16A C16 H16B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.313 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.323 # Attachment 's1290compound5_1.cif' data_e1290 _database_code_depnum_ccdc_archive 'CCDC 743174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H64 F12 N8 O8 S12 Si2 Zn2' _chemical_formula_sum 'C64 H64 F12 N8 O8 S12 Si2 Zn2' _chemical_formula_weight 1872.87 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1804(4) _cell_length_b 15.8350(5) _cell_length_c 28.8368(8) _cell_angle_alpha 99.985(2) _cell_angle_beta 94.883(2) _cell_angle_gamma 106.023(2) _cell_volume 5640.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9049 _exptl_absorpt_correction_T_max 0.9374 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied Because of the disorderthe atoms C57, C58, S12 and S13 have identical thermal parameters using the command EADP ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63726 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.1518 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.68 _reflns_number_total 25498 _reflns_number_gt 12679 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0703P)^2^+0.3124P] 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 25498 _refine_ls_number_parameters 950 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.1882 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.046 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 1.5000 1.0000 0.5000 0.01876(19) Uani 1 2 d S . . Zn2 Zn 1.26089(5) 0.75115(4) 0.24632(2) 0.02037(14) Uani 1 1 d . . . Zn3 Zn 1.0000 0.5000 0.0000 0.01966(19) Uani 1 2 d S . . Si1 Si 1.36722(12) 0.89096(11) 0.37084(5) 0.0227(3) Uani 1 1 d . . . F1 F 1.4195(2) 0.9451(2) 0.42856(10) 0.0277(7) Uani 1 1 d . . . F2 F 1.3164(2) 0.8360(2) 0.31339(9) 0.0272(7) Uani 1 1 d . . . F3 F 1.2991(3) 0.9642(3) 0.36544(12) 0.0468(10) Uani 1 1 d . . . F4 F 1.4702(3) 0.9564(2) 0.35145(11) 0.0359(8) Uani 1 1 d . . . F5 F 1.2647(3) 0.8248(2) 0.39003(11) 0.0420(9) Uani 1 1 d . . . F6 F 1.4339(3) 0.8168(2) 0.37424(10) 0.0315(8) Uani 1 1 d . . . Si2 Si 1.14979(11) 0.60377(10) 0.12358(5) 0.0194(3) Uani 1 1 d . . . F7 F 1.2039(2) 0.6603(2) 0.18074(9) 0.0234(7) Uani 1 1 d . . . F8 F 1.0928(2) 0.5483(2) 0.06691(9) 0.0266(7) Uani 1 1 d . . . F9 F 1.0655(2) 0.6627(2) 0.12406(11) 0.0311(7) Uani 1 1 d . . . F10 F 1.2382(3) 0.6791(2) 0.10262(10) 0.0345(8) Uani 1 1 d . . . F11 F 1.0627(3) 0.5268(2) 0.14560(10) 0.0331(8) Uani 1 1 d . . . F12 F 1.2323(3) 0.5411(2) 0.12455(12) 0.0396(9) Uani 1 1 d . . . N1 N 1.3495(3) 1.0004(3) 0.52375(14) 0.0221(10) Uani 1 1 d . . . C1 C 1.3443(4) 1.0603(4) 0.5616(2) 0.0347(15) Uani 1 1 d . . . H1 H 1.4072 1.1061 0.5769 0.042 Uiso 1 1 calc R . . C2 C 1.2497(5) 1.0564(5) 0.5788(2) 0.050(2) Uani 1 1 d . . . H2 H 1.2485 1.0979 0.6067 0.060 Uiso 1 1 calc R . . C3 C 1.1572(5) 0.9939(4) 0.5565(2) 0.0366(15) Uani 1 1 d . . . C4 C 1.1624(4) 0.9350(4) 0.5170(2) 0.0343(14) Uani 1 1 d . . . H4 H 1.0990 0.8923 0.4999 0.041 Uiso 1 1 calc R . . C5 C 1.2599(5) 0.9371(4) 0.5018(2) 0.0330(14) Uani 1 1 d . . . H5 H 1.2632 0.8932 0.4754 0.040 Uiso 1 1 calc R . . C6 C 1.0531(6) 0.9960(5) 0.5754(3) 0.055(2) Uani 1 1 d . . . O1 O 1.0538(4) 1.0538(4) 0.6080(3) 0.106(3) Uani 1 1 d . . . S1 S 0.94165(14) 0.91199(14) 0.54751(7) 0.0542(5) Uani 1 1 d . . . C7 C 0.8480(5) 0.9391(4) 0.5848(3) 0.0413(16) Uani 1 1 d . . . H7A H 0.8657 0.9293 0.6171 0.050 Uiso 1 1 calc R . . H7B H 0.8520 1.0032 0.5874 0.050 Uiso 1 1 calc R . . C8 C 0.7348(5) 0.8797(4) 0.5633(2) 0.0404(15) Uani 1 1 d . . . H8A H 0.7139 0.8981 0.5337 0.049 Uiso 1 1 calc R . . H8B H 0.6852 0.8912 0.5859 0.049 Uiso 1 1 calc R . . S2 S 0.7186(2) 0.76581(15) 0.55039(8) 0.0683(4) Uani 1 1 d . . . C9 C 0.7533(7) 0.7407(6) 0.6011(3) 0.0683(4) Uani 1 1 d . . . H9A H 0.7711 0.6835 0.5934 0.082 Uiso 1 1 calc R . . H9B H 0.8203 0.7874 0.6164 0.082 Uiso 1 1 calc R . . C10 C 0.6765(7) 0.7305(6) 0.6394(3) 0.0683(4) Uani 1 1 d . . . H10A H 0.6044 0.6949 0.6230 0.082 Uiso 1 1 calc R . . H10B H 0.6726 0.7910 0.6534 0.082 Uiso 1 1 calc R . . S3 S 0.7091(2) 0.67828(15) 0.68829(8) 0.0683(4) Uani 1 1 d . . . C11 C 0.6749(6) 0.5689(5) 0.6551(3) 0.056(2) Uani 1 1 d . . . O2 O 0.6372(5) 0.5465(4) 0.61297(19) 0.0672(17) Uani 1 1 d . . . C12 C 0.7000(5) 0.4991(4) 0.68139(19) 0.0326(14) Uani 1 1 d . . . C13 C 0.7195(5) 0.4255(4) 0.65509(19) 0.0383(15) Uani 1 1 d . . . H13 H 0.7220 0.4200 0.6219 0.046 Uiso 1 1 calc R . . C14 C 0.7350(5) 0.3608(4) 0.67781(19) 0.0304(13) Uani 1 1 d . . . H14 H 0.7489 0.3102 0.6596 0.036 Uiso 1 1 calc R . . N2 N 0.7318(4) 0.3640(3) 0.72390(15) 0.0252(10) Uani 1 1 d . . . C15 C 0.7130(5) 0.4380(4) 0.7499(2) 0.0351(14) Uani 1 1 d . . . H15 H 0.7104 0.4414 0.7830 0.042 Uiso 1 1 calc R . . C16 C 0.6981(6) 0.5067(4) 0.7304(2) 0.0428(17) Uani 1 1 d . . . H16 H 0.6868 0.5578 0.7493 0.051 Uiso 1 1 calc R . . N3 N 1.0982(3) 0.7315(3) 0.26083(15) 0.0226(10) Uani 1 1 d . . . C17 C 1.0720(5) 0.7942(4) 0.29174(19) 0.0318(13) Uani 1 1 d . . . H17 H 1.1256 0.8475 0.3077 0.038 Uiso 1 1 calc R . . C18 C 0.9671(5) 0.7812(4) 0.3002(2) 0.0335(14) Uani 1 1 d . . . H18 H 0.9486 0.8253 0.3218 0.040 Uiso 1 1 calc R . . C19 C 0.8890(5) 0.7021(4) 0.2765(2) 0.0323(14) Uani 1 1 d . . . C20 C 0.9191(5) 0.6393(4) 0.2452(2) 0.0346(14) Uani 1 1 d . . . H20 H 0.8679 0.5853 0.2284 0.041 Uiso 1 1 calc R . . C21 C 1.0248(5) 0.6571(4) 0.2391(2) 0.0328(14) Uani 1 1 d . . . H21 H 1.0457 0.6135 0.2183 0.039 Uiso 1 1 calc R . . C22 C 0.7746(5) 0.6802(5) 0.2837(2) 0.0454(17) Uani 1 1 d . . . O3 O 0.7058(4) 0.6125(4) 0.2620(2) 0.0700(17) Uani 1 1 d . . . S4 S 0.74336(16) 0.75425(15) 0.32800(8) 0.0666(6) Uani 1 1 d . . . C23 C 0.6012(6) 0.6959(6) 0.3283(3) 0.069(3) Uani 1 1 d . . . H23A H 0.5640 0.7403 0.3397 0.083 Uiso 1 1 calc R . . H23B H 0.5674 0.6645 0.2956 0.083 Uiso 1 1 calc R . . C24 C 0.5908(6) 0.6283(6) 0.3606(3) 0.064(2) Uani 1 1 d . . . H24A H 0.6394 0.5915 0.3535 0.077 Uiso 1 1 calc R . . H24B H 0.5168 0.5878 0.3552 0.077 Uiso 1 1 calc R . . S5 S 0.6255(2) 0.69069(15) 0.42353(9) 0.0705(7) Uani 1 1 d . . . C25 C 0.6086(7) 0.5971(6) 0.4543(3) 0.070(3) Uani 1 1 d . . . H25A H 0.5853 0.6136 0.4855 0.084 Uiso 1 1 calc R . . H25B H 0.5522 0.5442 0.4353 0.084 Uiso 1 1 calc R . . C26 C 0.7117(6) 0.5726(5) 0.4619(3) 0.067(2) Uani 1 1 d . . . H26A H 0.7689 0.6258 0.4800 0.080 Uiso 1 1 calc R . . H26B H 0.7337 0.5537 0.4308 0.080 Uiso 1 1 calc R . . S6 S 0.69402(19) 0.48333(14) 0.49395(8) 0.0630(6) Uani 1 1 d . . . C27 C 0.6265(5) 0.3924(4) 0.4484(2) 0.0393(15) Uani 1 1 d . . . O4 O 0.6053(5) 0.4012(3) 0.40748(17) 0.0626(15) Uani 1 1 d . . . C28 C 0.5968(5) 0.3028(4) 0.4623(2) 0.0305(13) Uani 1 1 d . . . C29 C 0.5690(5) 0.2249(4) 0.42669(19) 0.0340(14) Uani 1 1 d . . . H29 H 0.5701 0.2283 0.3942 0.041 Uiso 1 1 calc R . . C30 C 0.5404(5) 0.1441(4) 0.43993(19) 0.0310(13) Uani 1 1 d . . . H30 H 0.5230 0.0914 0.4157 0.037 Uiso 1 1 calc R . . N4 N 0.5351(4) 0.1341(3) 0.48444(15) 0.0256(10) Uani 1 1 d . . . C31 C 0.5606(5) 0.2081(4) 0.5189(2) 0.0300(13) Uani 1 1 d . . . H31 H 0.5583 0.2019 0.5510 0.036 Uiso 1 1 calc R . . C32 C 0.5901(5) 0.2930(4) 0.5089(2) 0.0310(13) Uani 1 1 d . . . H32 H 0.6058 0.3444 0.5339 0.037 Uiso 1 1 calc R . . N5 N 1.0230(4) 0.6340(3) -0.01495(16) 0.0262(10) Uani 1 1 d . . . C33 C 1.0960(5) 0.7050(4) 0.0128(2) 0.0326(14) Uani 1 1 d . . . H33 H 1.1374 0.6955 0.0390 0.039 Uiso 1 1 calc R . . C34 C 1.1143(5) 0.7926(4) 0.0051(2) 0.0361(15) Uani 1 1 d . . . H34 H 1.1669 0.8413 0.0256 0.043 Uiso 1 1 calc R . . C35 C 1.0552(5) 0.8070(4) -0.0326(2) 0.0384(15) Uani 1 1 d . . . C36 C 0.9817(5) 0.7345(4) -0.0613(2) 0.0392(15) Uani 1 1 d . . . H36 H 0.9393 0.7420 -0.0877 0.047 Uiso 1 1 calc R . . C37 C 0.9697(5) 0.6505(4) -0.0517(2) 0.0342(14) Uani 1 1 d . . . H37 H 0.9197 0.6008 -0.0728 0.041 Uiso 1 1 calc R . . C38 C 1.0703(6) 0.9026(4) -0.0380(2) 0.0424(17) Uani 1 1 d . . . O5 O 1.1171(5) 0.9649(3) -0.00631(17) 0.0651(16) Uani 1 1 d . . . S7 S 1.0185(2) 0.91363(14) -0.09531(7) 0.0645(6) Uani 1 1 d . . . C39 C 1.0430(7) 1.0382(5) -0.0809(3) 0.070(3) Uani 1 1 d . . . H39A H 0.9967 1.0543 -0.1046 0.084 Uiso 1 1 calc R . . H39B H 1.0212 1.0546 -0.0494 0.084 Uiso 1 1 calc R . . C40 C 1.1494(6) 1.0899(5) -0.0801(3) 0.060(2) Uani 1 1 d . . . H40A H 1.1667 1.0835 -0.1131 0.072 Uiso 1 1 calc R . . H40B H 1.1974 1.0659 -0.0615 0.072 Uiso 1 1 calc R . . S8 S 1.17452(17) 1.20589(13) -0.05537(7) 0.0566(5) Uani 1 1 d . . . C41 C 1.0879(5) 1.2393(4) -0.0966(2) 0.0341(14) Uani 1 1 d . . . H41A H 1.0133 1.2064 -0.0945 0.041 Uiso 1 1 calc R . . H41B H 1.0968 1.3040 -0.0852 0.041 Uiso 1 1 calc R . . C42 C 1.1017(5) 1.2260(5) -0.1465(2) 0.0360(14) Uani 1 1 d . . . H42A H 1.0534 1.2520 -0.1636 0.043 Uiso 1 1 calc R . . H42B H 1.0803 1.1607 -0.1601 0.043 Uiso 1 1 calc R . . S9 S 1.23673(14) 1.27580(13) -0.15684(8) 0.0541(5) Uani 1 1 d . . . C43 C 1.2602(5) 1.1863(5) -0.1932(3) 0.055(2) Uani 1 1 d . . . O6 O 1.1951(5) 1.1196(5) -0.2095(3) 0.140(4) Uani 1 1 d . . . C44 C 1.3740(5) 1.2065(4) -0.2055(2) 0.0335(14) Uani 1 1 d . . . C45 C 1.3916(5) 1.1521(5) -0.2452(2) 0.0476(18) Uani 1 1 d . . . H45 H 1.3346 1.1046 -0.2640 0.057 Uiso 1 1 calc R . . C46 C 1.4955(5) 1.1688(5) -0.2569(2) 0.0459(18) Uani 1 1 d . . . H46 H 1.5083 1.1353 -0.2853 0.055 Uiso 1 1 calc R . . N6 N 1.5764(4) 1.2314(3) -0.22853(15) 0.0242(10) Uani 1 1 d . . . C47 C 1.5605(4) 1.2787(4) -0.18912(19) 0.0283(13) Uani 1 1 d . . . H47 H 1.6199 1.3209 -0.1687 0.034 Uiso 1 1 calc R . . C48 C 1.4583(4) 1.2685(4) -0.1764(2) 0.0359(15) Uani 1 1 d . . . H48 H 1.4480 1.3040 -0.1481 0.043 Uiso 1 1 calc R . . N7 N 0.8567(4) 0.5026(3) 0.02905(15) 0.0278(11) Uani 1 1 d . . . C49 C 0.7736(5) 0.5172(4) 0.00485(19) 0.0342(14) Uani 1 1 d . . . H49 H 0.7788 0.5255 -0.0268 0.041 Uiso 1 1 calc R . . C50 C 0.6837(5) 0.5209(4) 0.0227(2) 0.0361(15) Uani 1 1 d . . . H50 H 0.6267 0.5304 0.0039 0.043 Uiso 1 1 calc R . . C51 C 0.6754(4) 0.5106(4) 0.06964(18) 0.0260(12) Uani 1 1 d . . . C52 C 0.7618(4) 0.4972(4) 0.09523(19) 0.0292(13) Uani 1 1 d . . . H52 H 0.7595 0.4895 0.1271 0.035 Uiso 1 1 calc R . . C53 C 0.8514(4) 0.4950(4) 0.07354(17) 0.0248(12) Uani 1 1 d . . . H53 H 0.9111 0.4878 0.0915 0.030 Uiso 1 1 calc R . . C54 C 0.5740(4) 0.5141(4) 0.0898(2) 0.0340(14) Uani 1 1 d . . . O7 O 0.5126(3) 0.5460(3) 0.07157(16) 0.0434(12) Uani 1 1 d . . . S10 S 0.55860(13) 0.46661(13) 0.14061(6) 0.0426(4) Uani 1 1 d . . . C55 C 0.4288(5) 0.4763(5) 0.1509(2) 0.0419(16) Uani 1 1 d . . . H55A H 0.4311 0.5007 0.1851 0.050 Uiso 1 1 calc R . . H55B H 0.4117 0.5197 0.1329 0.050 Uiso 1 1 calc R . . C56 C 0.3426(6) 0.3896(5) 0.1367(3) 0.0509(19) Uani 1 1 d . . . H56A H 0.2752 0.3986 0.1461 0.061 Uiso 1 1 calc R . . H56B H 0.3605 0.3456 0.1540 0.061 Uiso 1 1 calc R . . S11 S 0.32241(19) 0.34368(14) 0.07303(7) 0.0620(6) Uani 1 1 d . . . C57 C 0.2797(8) 0.2239(6) 0.0738(3) 0.0772(12) Uani 1 1 d . B . H57A H 0.2356 0.2164 0.0997 0.093 Uiso 1 1 calc R . . H57B H 0.2318 0.1932 0.0437 0.093 Uiso 1 1 calc R . . C58 C 0.3493(8) 0.1790(4) 0.0789(3) 0.0772(12) Uani 1 1 d D . . H58A H 0.4063 0.2103 0.1059 0.093 Uiso 1 1 calc R A 1 H58B H 0.3815 0.1674 0.0495 0.093 Uiso 1 1 calc R A 1 S12 S 0.2604(9) 0.0751(5) 0.0907(2) 0.0772(12) Uani 0.309(6) 1 d PD B 1 S13 S 0.3281(5) 0.0729(2) 0.09111(11) 0.0772(12) Uani 0.691(6) 1 d PD B 2 C59 C 0.3029(7) 0.0945(5) 0.15089(19) 0.060(2) Uani 1 1 d D . . O8 O 0.3174(6) 0.1694(3) 0.17487(19) 0.086(2) Uani 1 1 d . B . C60 C 0.2867(5) 0.0149(4) 0.1736(2) 0.0355(14) Uani 1 1 d . B . C61 C 0.2348(6) -0.0681(4) 0.1496(2) 0.0461(18) Uani 1 1 d . . . H61 H 0.2068 -0.0784 0.1170 0.055 Uiso 1 1 calc R B . C62 C 0.2218(6) -0.1400(5) 0.1732(2) 0.051(2) Uani 1 1 d . B . H62 H 0.1819 -0.1985 0.1563 0.062 Uiso 1 1 calc R . . N8 N 0.2626(3) -0.1300(3) 0.21773(15) 0.0256(10) Uani 1 1 d . . . C63 C 0.3110(7) -0.0467(5) 0.2409(2) 0.053(2) Uani 1 1 d . B . H63 H 0.3403 -0.0382 0.2732 0.064 Uiso 1 1 calc R . . C64 C 0.3215(7) 0.0260(5) 0.2222(3) 0.067(3) Uani 1 1 d . . . H64 H 0.3519 0.0844 0.2415 0.081 Uiso 1 1 calc R B . 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 0.0177(4) 0.0220(5) 0.0143(4) -0.0008(3) 0.0009(3) 0.0054(4) Zn2 0.0185(3) 0.0244(3) 0.0146(3) -0.0012(2) 0.0005(2) 0.0043(3) Zn3 0.0211(4) 0.0228(5) 0.0137(4) 0.0000(3) -0.0001(3) 0.0072(4) Si1 0.0229(7) 0.0258(9) 0.0137(6) -0.0043(6) -0.0003(6) 0.0040(7) F1 0.0275(17) 0.0315(19) 0.0168(15) -0.0010(13) -0.0002(13) 0.0017(15) F2 0.0282(17) 0.034(2) 0.0144(14) -0.0055(13) -0.0003(13) 0.0078(15) F3 0.060(2) 0.054(3) 0.0322(19) -0.0101(18) -0.0104(18) 0.043(2) F4 0.042(2) 0.0255(19) 0.0237(16) -0.0054(14) 0.0075(15) -0.0104(16) F5 0.037(2) 0.046(2) 0.0255(17) -0.0069(16) 0.0104(16) -0.0084(17) F6 0.0393(19) 0.032(2) 0.0222(16) -0.0017(14) -0.0093(14) 0.0169(16) Si2 0.0218(7) 0.0219(8) 0.0120(6) -0.0023(6) -0.0019(6) 0.0072(6) F7 0.0250(16) 0.0273(18) 0.0131(13) -0.0021(12) -0.0022(12) 0.0053(14) F8 0.0312(17) 0.0303(19) 0.0134(14) -0.0035(13) -0.0044(13) 0.0083(15) F9 0.0259(17) 0.0275(19) 0.0339(18) -0.0103(15) -0.0039(14) 0.0108(15) F10 0.0327(18) 0.038(2) 0.0206(15) 0.0061(15) -0.0016(14) -0.0067(16) F11 0.0386(19) 0.034(2) 0.0183(15) 0.0055(14) -0.0014(14) -0.0014(16) F12 0.038(2) 0.048(2) 0.0331(18) -0.0086(17) -0.0085(16) 0.0284(18) N1 0.022(2) 0.023(3) 0.016(2) -0.0044(18) -0.0042(18) 0.004(2) C1 0.016(3) 0.033(4) 0.041(3) -0.020(3) 0.001(2) 0.002(2) C2 0.025(3) 0.049(4) 0.053(4) -0.033(3) 0.007(3) -0.002(3) C3 0.026(3) 0.030(4) 0.051(4) -0.001(3) 0.015(3) 0.007(3) C4 0.016(3) 0.026(3) 0.048(4) -0.006(3) 0.004(3) -0.006(2) C5 0.044(4) 0.021(3) 0.029(3) -0.009(2) 0.013(3) 0.009(3) C6 0.051(4) 0.030(4) 0.074(5) -0.011(4) 0.040(4) 0.001(3) O1 0.050(4) 0.089(5) 0.141(6) -0.056(4) 0.066(4) -0.008(3) S1 0.0288(9) 0.0580(13) 0.0641(12) -0.0099(10) 0.0144(8) 0.0055(9) C7 0.027(3) 0.037(4) 0.066(4) 0.012(3) 0.019(3) 0.015(3) C8 0.036(4) 0.034(4) 0.050(4) 0.009(3) 0.008(3) 0.007(3) S2 0.0802(11) 0.0477(9) 0.0721(10) 0.0124(8) 0.0027(8) 0.0132(8) C9 0.0802(11) 0.0477(9) 0.0721(10) 0.0124(8) 0.0027(8) 0.0132(8) C10 0.0802(11) 0.0477(9) 0.0721(10) 0.0124(8) 0.0027(8) 0.0132(8) S3 0.0802(11) 0.0477(9) 0.0721(10) 0.0124(8) 0.0027(8) 0.0132(8) C11 0.051(4) 0.051(5) 0.070(5) 0.038(4) 0.007(4) 0.006(4) O2 0.092(4) 0.053(4) 0.052(3) 0.025(3) -0.017(3) 0.015(3) C12 0.035(3) 0.035(4) 0.022(3) 0.013(3) -0.004(2) 0.000(3) C13 0.050(4) 0.042(4) 0.015(3) 0.000(3) -0.002(3) 0.006(3) C14 0.039(3) 0.023(3) 0.024(3) 0.000(2) 0.007(3) 0.004(3) N2 0.028(2) 0.027(3) 0.020(2) 0.004(2) 0.0057(19) 0.008(2) C15 0.055(4) 0.031(4) 0.024(3) 0.005(3) 0.006(3) 0.020(3) C16 0.068(5) 0.037(4) 0.032(3) 0.009(3) 0.017(3) 0.025(4) N3 0.024(2) 0.023(3) 0.020(2) 0.0031(19) 0.0000(18) 0.009(2) C17 0.030(3) 0.034(4) 0.024(3) -0.008(3) -0.008(2) 0.007(3) C18 0.030(3) 0.037(4) 0.034(3) 0.000(3) 0.010(3) 0.013(3) C19 0.025(3) 0.048(4) 0.027(3) 0.009(3) 0.005(2) 0.015(3) C20 0.025(3) 0.035(4) 0.034(3) 0.000(3) -0.001(3) -0.001(3) C21 0.027(3) 0.032(4) 0.037(3) 0.005(3) 0.009(3) 0.005(3) C22 0.024(3) 0.061(5) 0.049(4) 0.007(4) 0.007(3) 0.012(3) O3 0.023(2) 0.072(4) 0.081(4) -0.021(3) 0.012(3) -0.020(3) S4 0.0438(11) 0.0629(14) 0.0778(14) -0.0170(11) 0.0297(11) 0.0040(10) C23 0.048(5) 0.084(7) 0.073(6) 0.022(5) 0.023(4) 0.007(5) C24 0.041(4) 0.065(6) 0.074(6) -0.012(5) 0.014(4) 0.010(4) S5 0.0997(18) 0.0448(13) 0.0895(16) 0.0292(12) 0.0440(15) 0.0393(13) C25 0.062(5) 0.059(6) 0.088(6) 0.007(5) 0.032(5) 0.016(5) C26 0.057(5) 0.038(5) 0.097(6) 0.002(4) 0.041(5) -0.002(4) S6 0.0780(15) 0.0339(11) 0.0691(13) 0.0116(10) -0.0023(12) 0.0069(10) C27 0.052(4) 0.034(4) 0.034(3) 0.013(3) 0.006(3) 0.011(3) O4 0.094(4) 0.050(3) 0.051(3) 0.027(3) 0.012(3) 0.023(3) C28 0.034(3) 0.026(3) 0.031(3) 0.011(3) 0.001(3) 0.007(3) C29 0.048(4) 0.034(4) 0.023(3) 0.006(3) 0.016(3) 0.014(3) C30 0.042(3) 0.029(3) 0.021(3) 0.003(2) 0.007(3) 0.009(3) N4 0.026(2) 0.028(3) 0.022(2) 0.001(2) -0.0017(19) 0.011(2) C31 0.040(3) 0.015(3) 0.035(3) 0.008(2) 0.000(3) 0.007(3) C32 0.036(3) 0.025(3) 0.033(3) 0.006(3) 0.003(3) 0.011(3) N5 0.031(3) 0.018(3) 0.025(2) -0.0018(19) -0.003(2) 0.006(2) C33 0.030(3) 0.034(4) 0.025(3) 0.001(3) -0.001(2) -0.001(3) C34 0.042(4) 0.031(4) 0.029(3) 0.005(3) 0.005(3) 0.001(3) C35 0.054(4) 0.031(4) 0.030(3) 0.009(3) 0.004(3) 0.011(3) C36 0.043(4) 0.032(4) 0.036(3) 0.006(3) -0.017(3) 0.006(3) C37 0.043(4) 0.023(3) 0.028(3) 0.000(3) -0.011(3) 0.004(3) C38 0.073(5) 0.029(4) 0.024(3) 0.004(3) 0.017(3) 0.010(3) O5 0.104(5) 0.036(3) 0.045(3) 0.012(3) 0.013(3) -0.001(3) S7 0.0962(17) 0.0377(12) 0.0527(11) 0.0161(9) -0.0127(11) 0.0113(11) C39 0.092(7) 0.053(6) 0.083(6) 0.035(5) 0.018(5) 0.037(5) C40 0.057(5) 0.046(5) 0.083(6) 0.037(5) 0.012(4) 0.011(4) S8 0.0627(13) 0.0390(11) 0.0565(11) 0.0126(9) -0.0203(10) 0.0034(10) C41 0.035(3) 0.027(3) 0.046(4) 0.015(3) 0.017(3) 0.009(3) C42 0.029(3) 0.043(4) 0.036(3) 0.010(3) 0.003(3) 0.010(3) S9 0.0328(9) 0.0444(11) 0.0765(13) -0.0083(10) 0.0239(9) 0.0053(8) C43 0.028(4) 0.062(5) 0.068(5) -0.007(4) 0.029(4) 0.007(4) O6 0.041(4) 0.102(6) 0.200(8) -0.096(5) 0.066(5) -0.038(4) C44 0.030(3) 0.024(3) 0.042(3) -0.003(3) 0.011(3) 0.004(3) C45 0.039(4) 0.035(4) 0.052(4) -0.025(3) 0.002(3) 0.005(3) C46 0.022(3) 0.060(5) 0.039(4) -0.016(3) -0.001(3) 0.003(3) N6 0.025(2) 0.023(3) 0.022(2) 0.0006(19) 0.0031(19) 0.006(2) C47 0.015(3) 0.039(4) 0.023(3) -0.001(3) -0.001(2) 0.001(2) C48 0.016(3) 0.046(4) 0.034(3) -0.004(3) 0.008(2) -0.003(3) N7 0.036(3) 0.031(3) 0.019(2) 0.007(2) 0.003(2) 0.014(2) C49 0.039(3) 0.049(4) 0.020(3) 0.012(3) -0.003(3) 0.021(3) C50 0.040(3) 0.053(4) 0.033(3) 0.020(3) 0.009(3) 0.034(3) C51 0.022(3) 0.037(4) 0.020(2) 0.006(2) 0.005(2) 0.008(3) C52 0.020(3) 0.047(4) 0.024(3) 0.012(3) 0.004(2) 0.013(3) C53 0.022(3) 0.034(3) 0.018(2) 0.004(2) 0.003(2) 0.007(2) C54 0.016(3) 0.050(4) 0.038(3) 0.010(3) 0.011(2) 0.010(3) O7 0.034(2) 0.060(3) 0.053(3) 0.023(3) 0.012(2) 0.032(2) S10 0.0344(8) 0.0688(13) 0.0354(8) 0.0230(9) 0.0116(7) 0.0235(9) C55 0.048(4) 0.050(5) 0.039(3) 0.013(3) 0.012(3) 0.028(4) C56 0.056(5) 0.046(5) 0.059(5) 0.023(4) 0.021(4) 0.018(4) S11 0.0860(16) 0.0402(12) 0.0594(12) 0.0193(10) -0.0117(11) 0.0187(11) C57 0.151(4) 0.0606(17) 0.0442(12) 0.0208(12) 0.022(2) 0.061(2) C58 0.151(4) 0.0606(17) 0.0442(12) 0.0208(12) 0.022(2) 0.061(2) S12 0.151(4) 0.0606(17) 0.0442(12) 0.0208(12) 0.022(2) 0.061(2) S13 0.151(4) 0.0606(17) 0.0442(12) 0.0208(12) 0.022(2) 0.061(2) C59 0.117(7) 0.032(4) 0.035(4) 0.016(3) 0.005(4) 0.027(5) O8 0.174(7) 0.025(3) 0.048(3) 0.007(2) 0.004(4) 0.018(4) C60 0.057(4) 0.020(3) 0.026(3) 0.002(2) -0.001(3) 0.009(3) C61 0.083(5) 0.022(4) 0.026(3) -0.003(3) -0.014(3) 0.015(4) C62 0.062(5) 0.035(4) 0.040(4) 0.007(3) -0.025(3) -0.004(4) N8 0.020(2) 0.028(3) 0.020(2) -0.001(2) -0.0054(18) 0.000(2) C63 0.091(6) 0.041(4) 0.013(3) -0.006(3) -0.014(3) 0.007(4) C64 0.110(7) 0.022(4) 0.042(4) 0.004(3) -0.025(4) -0.013(4) _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 F1 2.150(3) 2_876 ? Zn1 F1 2.150(3) . ? Zn1 N1 2.154(4) . ? Zn1 N1 2.154(4) 2_876 ? Zn1 N4 2.179(5) 2_766 ? Zn1 N4 2.179(5) 1_665 ? Zn2 F2 2.097(3) . ? Zn2 F7 2.104(3) . ? Zn2 N3 2.167(4) . ? Zn2 N2 2.168(4) 2_766 ? Zn2 N8 2.177(5) 1_665 ? Zn2 N6 2.202(4) 2_875 ? Zn3 F8 2.091(3) . ? Zn3 F8 2.091(3) 2_765 ? Zn3 N7 2.138(4) . ? Zn3 N7 2.139(4) 2_765 ? Zn3 N5 2.183(4) . ? Zn3 N5 2.183(4) 2_765 ? Si1 F6 1.661(3) . ? Si1 F5 1.666(3) . ? Si1 F4 1.668(3) . ? Si1 F3 1.670(4) . ? Si1 F2 1.714(3) . ? Si1 F1 1.721(3) . ? Si2 F9 1.636(3) . ? Si2 F10 1.658(3) . ? Si2 F12 1.664(4) . ? Si2 F11 1.681(3) . ? Si2 F8 1.714(3) . ? Si2 F7 1.721(3) . ? N1 C1 1.336(7) . ? N1 C5 1.341(7) . ? C1 C2 1.371(8) . ? C1 H1 0.9500 . ? C2 C3 1.363(8) . ? C2 H2 0.9500 . ? C3 C4 1.360(8) . ? C3 C6 1.525(8) . ? C4 C5 1.387(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 O1 1.191(8) . ? C6 S1 1.710(8) . ? S1 C7 1.794(6) . ? C7 C8 1.536(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 S2 1.726(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? S2 C9 1.640(8) . ? C9 C10 1.561(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 S3 1.831(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? S3 C11 1.744(9) . ? C11 O2 1.223(9) . ? C11 C12 1.536(8) . ? C12 C13 1.375(9) . ? C12 C16 1.402(7) . ? C13 C14 1.360(8) . ? C13 H13 0.9500 . ? C14 N2 1.326(6) . ? C14 H14 0.9500 . ? N2 C15 1.372(7) . ? N2 Zn2 2.168(4) 2_766 ? C15 C16 1.359(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N3 C21 1.315(7) . ? N3 C17 1.355(7) . ? C17 C18 1.389(8) . ? C17 H17 0.9500 . ? C18 C19 1.403(8) . ? C18 H18 0.9500 . ? C19 C20 1.390(8) . ? C19 C22 1.491(8) . ? C20 C21 1.376(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O3 1.223(8) . ? C22 S4 1.737(7) . ? S4 C23 1.848(7) . ? C23 C24 1.522(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 S5 1.862(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? S5 C25 1.828(8) . ? C25 C26 1.522(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 S6 1.792(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? S6 C27 1.739(7) . ? C27 O4 1.231(7) . ? C27 C28 1.497(8) . ? C28 C32 1.389(7) . ? C28 C29 1.399(8) . ? C29 C30 1.361(8) . ? C29 H29 0.9500 . ? C30 N4 1.326(6) . ? C30 H30 0.9500 . ? N4 C31 1.339(7) . ? N4 Zn1 2.179(5) 1_445 ? C31 C32 1.380(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? N5 C37 1.324(7) . ? N5 C33 1.338(7) . ? C33 C34 1.402(8) . ? C33 H33 0.9500 . ? C34 C35 1.372(8) . ? C34 H34 0.9500 . ? C35 C36 1.364(9) . ? C35 C38 1.509(8) . ? C36 C37 1.376(8) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 O5 1.201(8) . ? C38 S7 1.789(7) . ? S7 C39 1.873(8) . ? C39 C40 1.412(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 S8 1.778(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? S8 C41 1.822(6) . ? C41 C42 1.452(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 S9 1.810(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? S9 C43 1.727(7) . ? C43 O6 1.155(9) . ? C43 C44 1.530(8) . ? C44 C48 1.362(8) . ? C44 C45 1.386(8) . ? C45 C46 1.405(8) . ? C45 H45 0.9500 . ? C46 N6 1.333(7) . ? C46 H46 0.9500 . ? N6 C47 1.315(7) . ? N6 Zn2 2.202(4) 2_875 ? C47 C48 1.400(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N7 C53 1.315(6) . ? N7 C49 1.344(7) . ? C49 C50 1.344(8) . ? C49 H49 0.9500 . ? C50 C51 1.401(7) . ? C50 H50 0.9500 . ? C51 C52 1.389(7) . ? C51 C54 1.514(7) . ? C52 C53 1.389(7) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 O7 1.197(7) . ? C54 S10 1.760(6) . ? S10 C55 1.804(6) . ? C55 C56 1.487(9) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 S11 1.821(8) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? S11 C57 1.829(8) . ? C57 C58 1.319(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 S13 1.730(6) . ? C58 S12 1.843(8) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? S12 C59 1.724(7) . ? S13 C59 1.776(6) . ? C59 O8 1.220(8) . ? C59 C60 1.491(8) . ? C60 C61 1.335(8) . ? C60 C64 1.404(8) . ? C61 C62 1.404(8) . ? C61 H61 0.9500 . ? C62 N8 1.314(7) . ? C62 H62 0.9500 . ? N8 C63 1.323(8) . ? N8 Zn2 2.177(5) 1_445 ? C63 C64 1.334(9) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? 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 F1 Zn1 F1 179.999(1) 2_876 . ? F1 Zn1 N1 90.43(13) 2_876 . ? F1 Zn1 N1 89.57(14) . . ? F1 Zn1 N1 89.58(14) 2_876 2_876 ? F1 Zn1 N1 90.42(13) . 2_876 ? N1 Zn1 N1 179.994(1) . 2_876 ? F1 Zn1 N4 89.38(14) 2_876 2_766 ? F1 Zn1 N4 90.62(14) . 2_766 ? N1 Zn1 N4 85.03(16) . 2_766 ? N1 Zn1 N4 94.97(16) 2_876 2_766 ? F1 Zn1 N4 90.62(14) 2_876 1_665 ? F1 Zn1 N4 89.38(14) . 1_665 ? N1 Zn1 N4 94.97(16) . 1_665 ? N1 Zn1 N4 85.03(16) 2_876 1_665 ? N4 Zn1 N4 180.0(2) 2_766 1_665 ? F2 Zn2 F7 177.05(12) . . ? F2 Zn2 N3 89.82(14) . . ? F7 Zn2 N3 89.56(14) . . ? F2 Zn2 N2 90.57(15) . 2_766 ? F7 Zn2 N2 86.55(14) . 2_766 ? N3 Zn2 N2 90.24(16) . 2_766 ? F2 Zn2 N8 87.85(15) . 1_665 ? F7 Zn2 N8 95.05(14) . 1_665 ? N3 Zn2 N8 92.37(16) . 1_665 ? N2 Zn2 N8 176.94(17) 2_766 1_665 ? F2 Zn2 N6 92.45(15) . 2_875 ? F7 Zn2 N6 88.19(14) . 2_875 ? N3 Zn2 N6 177.67(17) . 2_875 ? N2 Zn2 N6 90.24(16) 2_766 2_875 ? N8 Zn2 N6 87.22(16) 1_665 2_875 ? F8 Zn3 F8 179.999(1) . 2_765 ? F8 Zn3 N7 92.31(14) . . ? F8 Zn3 N7 87.69(14) 2_765 . ? F8 Zn3 N7 87.70(14) . 2_765 ? F8 Zn3 N7 92.30(14) 2_765 2_765 ? N7 Zn3 N7 180.0 . 2_765 ? F8 Zn3 N5 93.49(15) . . ? F8 Zn3 N5 86.51(15) 2_765 . ? N7 Zn3 N5 91.70(17) . . ? N7 Zn3 N5 88.30(17) 2_765 . ? F8 Zn3 N5 86.52(15) . 2_765 ? F8 Zn3 N5 93.48(15) 2_765 2_765 ? N7 Zn3 N5 88.30(17) . 2_765 ? N7 Zn3 N5 91.71(17) 2_765 2_765 ? N5 Zn3 N5 179.998(1) . 2_765 ? F6 Si1 F5 89.69(19) . . ? F6 Si1 F4 89.82(19) . . ? F5 Si1 F4 179.5(2) . . ? F6 Si1 F3 178.05(18) . . ? F5 Si1 F3 90.7(2) . . ? F4 Si1 F3 89.8(2) . . ? F6 Si1 F2 88.55(16) . . ? F5 Si1 F2 89.91(17) . . ? F4 Si1 F2 89.87(16) . . ? F3 Si1 F2 89.53(17) . . ? F6 Si1 F1 90.58(16) . . ? F5 Si1 F1 90.19(16) . . ? F4 Si1 F1 90.03(16) . . ? F3 Si1 F1 91.33(17) . . ? F2 Si1 F1 179.13(19) . . ? Si1 F1 Zn1 171.4(2) . . ? Si1 F2 Zn2 170.7(2) . . ? F9 Si2 F10 91.85(18) . . ? F9 Si2 F12 177.47(19) . . ? F10 Si2 F12 90.61(19) . . ? F9 Si2 F11 89.36(18) . . ? F10 Si2 F11 178.6(2) . . ? F12 Si2 F11 88.17(19) . . ? F9 Si2 F8 89.41(17) . . ? F10 Si2 F8 90.74(16) . . ? F12 Si2 F8 91.13(17) . . ? F11 Si2 F8 90.06(16) . . ? F9 Si2 F7 89.13(16) . . ? F10 Si2 F7 89.88(16) . . ? F12 Si2 F7 90.31(17) . . ? F11 Si2 F7 89.35(15) . . ? F8 Si2 F7 178.43(17) . . ? Si2 F7 Zn2 168.32(19) . . ? Si2 F8 Zn3 166.50(19) . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Zn1 121.0(4) . . ? C5 N1 Zn1 119.9(3) . . ? N1 C1 C2 121.0(5) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 121.0(6) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 117.7(5) . . ? C4 C3 C6 123.3(6) . . ? C2 C3 C6 118.9(6) . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 120.9(5) . . ? N1 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? O1 C6 C3 119.5(7) . . ? O1 C6 S1 124.4(5) . . ? C3 C6 S1 116.1(5) . . ? C6 S1 C7 98.6(3) . . ? C8 C7 S1 109.6(5) . . ? C8 C7 H7A 109.8 . . ? S1 C7 H7A 109.8 . . ? C8 C7 H7B 109.8 . . ? S1 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C7 C8 S2 115.3(5) . . ? C7 C8 H8A 108.4 . . ? S2 C8 H8A 108.5 . . ? C7 C8 H8B 108.4 . . ? S2 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C9 S2 C8 105.4(4) . . ? C10 C9 S2 121.2(7) . . ? C10 C9 H9A 107.0 . . ? S2 C9 H9A 107.0 . . ? C10 C9 H9B 107.0 . . ? S2 C9 H9B 107.0 . . ? H9A C9 H9B 106.7 . . ? C9 C10 S3 117.6(6) . . ? C9 C10 H10A 107.9 . . ? S3 C10 H10A 107.9 . . ? C9 C10 H10B 107.9 . . ? S3 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? C11 S3 C10 96.6(4) . . ? O2 C11 C12 119.7(7) . . ? O2 C11 S3 124.6(6) . . ? C12 C11 S3 115.6(6) . . ? C13 C12 C16 120.1(5) . . ? C13 C12 C11 118.1(6) . . ? C16 C12 C11 121.7(6) . . ? C14 C13 C12 118.3(5) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N2 C14 C13 123.9(6) . . ? N2 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C14 N2 C15 117.5(5) . . ? C14 N2 Zn2 119.7(4) . 2_766 ? C15 N2 Zn2 122.5(3) . 2_766 ? C16 C15 N2 122.9(5) . . ? C16 C15 H15 118.6 . . ? N2 C15 H15 118.6 . . ? C15 C16 C12 117.4(6) . . ? C15 C16 H16 121.3 . . ? C12 C16 H16 121.3 . . ? C21 N3 C17 120.2(5) . . ? C21 N3 Zn2 118.8(4) . . ? C17 N3 Zn2 121.1(4) . . ? N3 C17 C18 120.4(6) . . ? N3 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 119.1(5) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 118.8(5) . . ? C20 C19 C22 117.5(6) . . ? C18 C19 C22 123.7(6) . . ? C21 C20 C19 118.4(6) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? N3 C21 C20 123.1(6) . . ? N3 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? O3 C22 C19 123.8(6) . . ? O3 C22 S4 120.2(5) . . ? C19 C22 S4 115.9(5) . . ? C22 S4 C23 100.9(4) . . ? C24 C23 S4 110.1(6) . . ? C24 C23 H23A 109.6 . . ? S4 C23 H23A 109.6 . . ? C24 C23 H23B 109.7 . . ? S4 C23 H23B 109.7 . . ? H23A C23 H23B 108.1 . . ? C23 C24 S5 108.7(6) . . ? C23 C24 H24A 110.0 . . ? S5 C24 H24A 110.0 . . ? C23 C24 H24B 109.9 . . ? S5 C24 H24B 110.0 . . ? H24A C24 H24B 108.3 . . ? C25 S5 C24 100.3(4) . . ? C26 C25 S5 111.4(5) . . ? C26 C25 H25A 109.3 . . ? S5 C25 H25A 109.3 . . ? C26 C25 H25B 109.4 . . ? S5 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 S6 110.5(5) . . ? C25 C26 H26A 109.6 . . ? S6 C26 H26A 109.6 . . ? C25 C26 H26B 109.5 . . ? S6 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C27 S6 C26 100.0(4) . . ? O4 C27 C28 122.3(6) . . ? O4 C27 S6 122.1(5) . . ? C28 C27 S6 115.6(4) . . ? C32 C28 C29 117.9(5) . . ? C32 C28 C27 122.9(6) . . ? C29 C28 C27 119.1(5) . . ? C30 C29 C28 118.2(5) . . ? C30 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? N4 C30 C29 124.3(6) . . ? N4 C30 H30 117.8 . . ? C29 C30 H30 117.8 . . ? C30 N4 C31 118.1(5) . . ? C30 N4 Zn1 119.5(4) . 1_445 ? C31 N4 Zn1 122.1(3) . 1_445 ? N4 C31 C32 121.8(5) . . ? N4 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C31 C32 C28 119.6(6) . . ? C31 C32 H32 120.2 . . ? C28 C32 H32 120.2 . . ? C37 N5 C33 116.0(5) . . ? C37 N5 Zn3 123.6(4) . . ? C33 N5 Zn3 120.4(4) . . ? N5 C33 C34 123.0(6) . . ? N5 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C35 C34 C33 119.0(6) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C36 C35 C34 118.0(6) . . ? C36 C35 C38 123.9(6) . . ? C34 C35 C38 118.0(6) . . ? C35 C36 C37 119.4(6) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? N5 C37 C36 124.5(6) . . ? N5 C37 H37 117.7 . . ? C36 C37 H37 117.7 . . ? O5 C38 C35 121.3(6) . . ? O5 C38 S7 124.2(5) . . ? C35 C38 S7 114.4(5) . . ? C38 S7 C39 97.1(4) . . ? C40 C39 S7 115.2(6) . . ? C40 C39 H39A 108.5 . . ? S7 C39 H39A 108.5 . . ? C40 C39 H39B 108.5 . . ? S7 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C39 C40 S8 113.6(6) . . ? C39 C40 H40A 108.8 . . ? S8 C40 H40A 108.8 . . ? C39 C40 H40B 108.9 . . ? S8 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C40 S8 C41 102.3(3) . . ? C42 C41 S8 118.6(4) . . ? C42 C41 H41A 107.7 . . ? S8 C41 H41A 107.7 . . ? C42 C41 H41B 107.7 . . ? S8 C41 H41B 107.6 . . ? H41A C41 H41B 107.1 . . ? C41 C42 S9 113.7(4) . . ? C41 C42 H42A 108.8 . . ? S9 C42 H42A 108.8 . . ? C41 C42 H42B 108.8 . . ? S9 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C43 S9 C42 101.3(3) . . ? O6 C43 C44 122.5(6) . . ? O6 C43 S9 123.7(5) . . ? C44 C43 S9 113.5(5) . . ? C48 C44 C45 119.7(6) . . ? C48 C44 C43 122.5(6) . . ? C45 C44 C43 117.4(6) . . ? C44 C45 C46 118.5(6) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.8 . . ? N6 C46 C45 120.4(6) . . ? N6 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C47 N6 C46 120.8(5) . . ? C47 N6 Zn2 120.3(4) . 2_875 ? C46 N6 Zn2 118.9(4) . 2_875 ? N6 C47 C48 121.8(5) . . ? N6 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C44 C48 C47 118.5(6) . . ? C44 C48 H48 120.8 . . ? C47 C48 H48 120.8 . . ? C53 N7 C49 118.0(5) . . ? C53 N7 Zn3 118.9(4) . . ? C49 N7 Zn3 123.0(3) . . ? C50 C49 N7 124.0(5) . . ? C50 C49 H49 118.0 . . ? N7 C49 H49 118.0 . . ? C49 C50 C51 118.8(5) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C52 C51 C50 117.6(5) . . ? C52 C51 C54 123.4(4) . . ? C50 C51 C54 119.0(5) . . ? C53 C52 C51 119.1(5) . . ? C53 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? N7 C53 C52 122.5(5) . . ? N7 C53 H53 118.8 . . ? C52 C53 H53 118.8 . . ? O7 C54 C51 121.1(5) . . ? O7 C54 S10 125.8(4) . . ? C51 C54 S10 113.1(4) . . ? C54 S10 C55 99.7(3) . . ? C56 C55 S10 113.3(5) . . ? C56 C55 H55A 108.9 . . ? S10 C55 H55A 108.9 . . ? C56 C55 H55B 108.9 . . ? S10 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 S11 112.8(4) . . ? C55 C56 H56A 109.0 . . ? S11 C56 H56A 109.0 . . ? C55 C56 H56B 109.0 . . ? S11 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? C56 S11 C57 99.5(3) . . ? C58 C57 S11 121.5(8) . . ? C58 C57 H57A 106.6 . . ? S11 C57 H57A 107.3 . . ? C58 C57 H57B 106.5 . . ? S11 C57 H57B 107.3 . . ? H57A C57 H57B 106.9 . . ? C57 C58 S13 128.6(7) . . ? C57 C58 S12 99.6(7) . . ? S13 C58 S12 29.0(3) . . ? C57 C58 H58A 111.3 . . ? S13 C58 H58A 96.5 . . ? S12 C58 H58A 111.8 . . ? C57 C58 H58B 111.8 . . ? S13 C58 H58B 96.9 . . ? S12 C58 H58B 112.3 . . ? H58A C58 H58B 109.8 . . ? C59 S12 C58 97.6(5) . . ? C58 S13 C59 99.9(4) . . ? O8 C59 C60 120.7(5) . . ? O8 C59 S12 118.9(6) . . ? C60 C59 S12 117.4(6) . . ? O8 C59 S13 124.3(5) . . ? C60 C59 S13 113.5(5) . . ? S12 C59 S13 29.8(3) . . ? C61 C60 C64 117.5(6) . . ? C61 C60 C59 122.2(6) . . ? C64 C60 C59 120.3(6) . . ? C60 C61 C62 119.2(6) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? N8 C62 C61 122.8(6) . . ? N8 C62 H62 118.6 . . ? C61 C62 H62 118.6 . . ? C62 N8 C63 116.5(5) . . ? C62 N8 Zn2 119.0(4) . 1_445 ? C63 N8 Zn2 124.2(4) . 1_445 ? N8 C63 C64 124.7(6) . . ? N8 C63 H63 117.6 . . ? C64 C63 H63 117.7 . . ? C63 C64 C60 118.8(6) . . ? C63 C64 H64 120.6 . . ? C60 C64 H64 120.6 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.260 _refine_diff_density_min -1.516 _refine_diff_density_rms 0.113 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.287 0.213 0.213 2184.0 1025.7 _platon_squeeze_details ; ;