# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 # 1. SUBMISSION DETAILS _publ_contact_author ; A. Monge Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; _publ_contact_author_phone '34 1 334-9025' _publ_contact_author_fax '34 1 372-0623' _publ_contact_author_email amonge@icmm.csic.es _publ_requested_coeditor_name ? _publ_contact_letter ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; One Teflon®-like Channelled Nanoporous Polymer with a Chiral and New Uninodal 4-connected Net. Sorption and catalityc properties. ; loop_ _publ_author_name _publ_author_address 'Angeles Monge' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Natalia Snejko' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Enrique Gutierrez-Puebla' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Manuela Medina' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Concepcion Cascales' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; ; C.Ruiz-Valero ; ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Marta Iglesias' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Berta Gomez-Lor' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; _publ_contact_author_name 'A. Monge' #============================================================================== data_zn1hept120 _database_code_depnum_ccdc_archive 'CCDC 226851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17.83 H8 F6 O4 Zn' _chemical_formula_sum 'C17.83 H8 F6 O4 Zn' _chemical_formula_weight 465.61 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' F F 0.0171 0.0103 '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 Hexagonal _symmetry_space_group_name_H-M P6(4)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z' 'y, -x+y, z+1/3' 'x-y, x, z+2/3' 'y, x, -z+1/3' 'x-y, -y, -z' '-x, -x+y, -z+2/3' '-y, -x, -z+1/3' '-x+y, y, -z' 'x, x-y, -z+2/3' _cell_length_a 21.155(3) _cell_length_b 21.155(3) _cell_length_c 7.6632(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2970.0(7) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 910 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 22.83 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1386 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 24432 _diffrn_reflns_av_R_equivalents 0.1373 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.75 _reflns_number_total 2464 _reflns_number_gt 2207 _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 performed with diffraction data from a crystal after treatement with heptane for several hours, and thus, of not very good quality.Data are good enough to locate some electron density in the channels of the structure, as a poof of the heptane insertion. 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^)+(0.0499P)^2^+21.8670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 2464 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1410 _refine_ls_R_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.2061 _refine_ls_wR_factor_gt 0.2000 _refine_ls_goodness_of_fit_ref 1.272 _refine_ls_restrained_S_all 1.272 _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 0.70023(4) 0.40046(7) 0.0000 0.0136(3) Uani 1 2 d S . . O2 O 0.7601(3) 0.3613(3) 0.0788(8) 0.0256(14) Uani 1 1 d . . . O1 O 0.7582(3) 0.4644(3) -0.1852(8) 0.0296(15) Uani 1 1 d . . . F1 F 0.9286(4) 0.2281(4) 0.5916(11) 0.058(2) Uani 1 1 d . . . F3 F 0.9977(4) 0.1838(3) 0.5304(13) 0.080(3) Uani 1 1 d . . . C1 C 0.7811(5) 0.3231(5) -0.0058(14) 0.027(2) Uani 1 1 d . . . C3 C 0.8372(4) 0.3105(4) 0.0845(13) 0.0199(19) Uani 1 1 d . . . F2 F 0.9012(4) 0.1530(3) 0.3803(13) 0.076(3) Uani 1 1 d . . . C4 C 0.8653(5) 0.2729(5) -0.0025(16) 0.031(2) Uani 1 1 d . . . H4 H 0.8491 0.2558 -0.1147 0.038 Uiso 1 1 calc R . . C8 C 1.0000 0.2731(6) 0.3333 0.039(4) Uani 1 2 d S . . C7 C 0.9142(5) 0.3235(5) 0.3299(16) 0.029(2) Uani 1 1 d . . . H7 H 0.9298 0.3399 0.4429 0.035 Uiso 1 1 calc R . . C9 C 0.9566(6) 0.2101(5) 0.462(2) 0.050(4) Uani 1 1 d . . . C6 C 0.9427(5) 0.2860(4) 0.2375(15) 0.027(2) Uani 1 1 d . . . C2 C 0.8620(5) 0.3359(5) 0.2497(13) 0.025(2) Uani 1 1 d . . . H2 H 0.8438 0.3617 0.3092 0.030 Uiso 1 1 calc R . . C5 C 0.9173(5) 0.2602(5) 0.0739(15) 0.031(2) Uani 1 1 d . . . H5 H 0.9350 0.2341 0.0136 0.038 Uiso 1 1 calc R . . C10 C 0.979(3) 0.0000 0.5000 0.090 Uiso 0.36(4) 2 d SP . . C11 C 1.0000 0.030(3) 0.3333 0.090 Uiso 0.31(4) 2 d SP . . 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(4) 0.0166(7) 0.0167(5) 0.000 0.0014(5) 0.0083(3) O2 0.015(3) 0.032(4) 0.034(3) -0.002(3) -0.007(3) 0.015(3) O1 0.034(4) 0.029(4) 0.025(3) 0.017(3) 0.015(3) 0.015(3) F1 0.035(4) 0.033(4) 0.089(6) 0.022(4) -0.017(4) 0.005(3) F3 0.055(4) 0.016(3) 0.164(8) 0.003(4) -0.064(6) 0.015(3) C1 0.019(4) 0.013(4) 0.046(5) 0.012(5) -0.003(5) 0.006(3) C3 0.007(4) 0.013(4) 0.040(5) -0.008(4) -0.011(4) 0.005(3) F2 0.042(4) 0.011(3) 0.154(9) -0.003(4) -0.064(5) -0.001(3) C4 0.016(4) 0.030(5) 0.048(6) -0.007(5) -0.014(5) 0.012(4) C8 0.027(7) 0.021(5) 0.070(11) -0.016(4) -0.031(8) 0.013(4) C7 0.022(5) 0.019(4) 0.042(5) -0.011(5) -0.021(5) 0.008(4) C9 0.037(7) 0.012(5) 0.087(11) -0.004(6) -0.047(7) 0.003(5) C6 0.016(4) 0.006(4) 0.055(6) -0.008(4) -0.021(4) 0.003(4) C2 0.019(5) 0.015(4) 0.039(5) 0.000(4) -0.003(4) 0.007(4) C5 0.025(5) 0.022(5) 0.052(7) -0.022(5) -0.021(5) 0.015(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 O1 1.921(6) . ? Zn1 O1 1.921(6) 11_655 ? Zn1 O2 1.925(6) . ? Zn1 O2 1.925(6) 11_655 ? O2 C1 1.275(11) . ? O1 C1 1.229(12) 12_554 ? F1 C9 1.305(16) . ? F3 C9 1.349(12) . ? C1 O1 1.229(12) 12_554 ? C1 C3 1.509(11) . ? C3 C2 1.373(13) . ? C3 C4 1.380(13) . ? F2 C9 1.347(11) . ? C4 C5 1.386(12) . ? C8 C9 1.540(15) 9_765 ? C8 C9 1.540(15) . ? C8 C6 1.555(11) . ? C8 C6 1.555(11) 9_765 ? C7 C2 1.397(13) . ? C7 C6 1.405(14) . ? C6 C5 1.365(13) . ? C10 C10 0.87(13) 4_755 ? C10 C11 1.39(2) 2_645 ? C10 C11 1.39(2) . ? C10 C11 1.58(4) 5_665 ? C10 C11 1.58(4) 4_755 ? C11 C11 1.26(14) 4_755 ? C11 C10 1.39(2) 3_764 ? C11 C10 1.58(4) 6_544 ? C11 C10 1.58(4) 4_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 104.8(4) . 11_655 ? O1 Zn1 O2 102.1(3) . . ? O1 Zn1 O2 104.2(3) 11_655 . ? O1 Zn1 O2 104.2(3) . 11_655 ? O1 Zn1 O2 102.1(3) 11_655 11_655 ? O2 Zn1 O2 136.3(4) . 11_655 ? C1 O2 Zn1 128.7(6) . . ? C1 O1 Zn1 136.5(6) 12_554 . ? O1 C1 O2 126.7(8) 12_554 . ? O1 C1 C3 117.6(8) 12_554 . ? O2 C1 C3 115.6(9) . . ? C2 C3 C4 118.7(8) . . ? C2 C3 C1 122.3(8) . . ? C4 C3 C1 119.0(9) . . ? C3 C4 C5 121.3(10) . . ? C9 C8 C9 111.1(14) 9_765 . ? C9 C8 C6 111.4(6) 9_765 . ? C9 C8 C6 106.0(5) . . ? C9 C8 C6 106.0(5) 9_765 9_765 ? C9 C8 C6 111.4(6) . 9_765 ? C6 C8 C6 111.0(10) . 9_765 ? C2 C7 C6 119.1(10) . . ? F1 C9 F2 107.3(11) . . ? F1 C9 F3 108.0(11) . . ? F2 C9 F3 105.1(8) . . ? F1 C9 C8 113.4(9) . . ? F2 C9 C8 110.5(10) . . ? F3 C9 C8 112.1(10) . . ? C5 C6 C7 119.6(9) . . ? C5 C6 C8 123.3(8) . . ? C7 C6 C8 117.0(8) . . ? C3 C2 C7 121.0(9) . . ? C6 C5 C4 120.1(10) . . ? C10 C10 C11 85(3) 4_755 2_645 ? C10 C10 C11 85(3) 4_755 . ? C11 C10 C11 170(6) 2_645 . ? C10 C10 C11 62(2) 4_755 5_665 ? C11 C10 C11 50(5) 2_645 5_665 ? C11 C10 C11 124(4) . 5_665 ? C10 C10 C11 62(2) 4_755 4_755 ? C11 C10 C11 124(4) 2_645 4_755 ? C11 C10 C11 50(5) . 4_755 ? C11 C10 C11 123(4) 5_665 4_755 ? C11 C11 C10 73(3) 4_755 3_764 ? C11 C11 C10 73(3) 4_755 . ? C10 C11 C10 146(7) 3_764 . ? C11 C11 C10 58(2) 4_755 6_544 ? C10 C11 C10 33(5) 3_764 6_544 ? C10 C11 C10 121(4) . 6_544 ? C11 C11 C10 58(2) 4_755 4_755 ? C10 C11 C10 121(4) 3_764 4_755 ? C10 C11 C10 33(5) . 4_755 ? C10 C11 C10 115(4) 6_544 4_755 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.024 _refine_diff_density_min -1.525 _refine_diff_density_rms 0.129 #============================================================================== data_zn1hept120 _database_code_depnum_ccdc_archive 'CCDC 253973' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17.17 H8 F6 O4 Zn' _chemical_formula_sum 'C17.17 H8 F6 O4 Zn' _chemical_formula_weight 457.61 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 21.224(10) _cell_length_b 21.224(10) _cell_length_c 7.710(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3008(3) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 910 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 22.83 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 24862 _diffrn_reflns_av_R_equivalents 0.1230 _diffrn_reflns_av_sigmaI/netI 0.1527 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.62 _reflns_number_total 8518 _reflns_number_gt 6226 _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^)+(0.0771P)^2^+5.4709P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 8518 _refine_ls_number_parameters 505 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.1063 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.005 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 O5 O 0.0917(4) 0.1315(4) 1.2984(10) 0.0318(19) Uani 1 1 d . A 1 O4 O 0.5757(4) 0.2025(4) 0.2971(10) 0.0303(19) Uani 1 1 d . B 1 Zn1 Zn 0.63313(6) 0.36689(6) 0.14908(14) 0.0155(3) Uani 1 1 d . . 1 Zn2 Zn 0.03347(6) -0.03350(6) 1.14879(14) 0.0155(3) Uani 1 1 d . . 1 C1 C 0.5527(6) 0.2095(7) 0.1543(16) 0.027(3) Uani 1 1 d . B 1 C23 C -0.1245(6) -0.1152(6) 1.1435(16) 0.026(3) Uani 1 1 d . C 1 C8 C 0.5524(6) 0.3430(6) 0.4786(16) 0.026(3) Uani 1 1 d . A 1 O8 O -0.0658(4) -0.0935(4) 1.2274(9) 0.0262(17) Uani 1 1 d . C 1 C22 C 0.1146(6) 0.1250(6) 1.1527(16) 0.024(3) Uani 1 1 d . A 1 O2 O 0.5749(5) 0.3724(4) 0.3349(11) 0.034(2) Uani 1 1 d . A 1 O3 O 0.5728(4) 0.3055(4) 0.5609(10) 0.0279(18) Uani 1 1 d . A 1 O7 O 0.0928(4) 0.0653(4) 1.0713(10) 0.0260(17) Uani 1 1 d . A 1 O1 O 0.5736(4) 0.2680(4) 0.0712(10) 0.0276(18) Uani 1 1 d . B 1 O6 O -0.1315(4) -0.0915(4) 1.0013(10) 0.0289(18) Uani 1 1 d . . 1 C9 C 0.4959(5) 0.3565(5) 0.5660(14) 0.021(2) Uani 1 1 d . A 1 C24 C -0.1933(5) -0.1704(5) 1.2329(14) 0.020(2) Uani 1 1 d . C 1 C2 C 0.4965(5) 0.1401(5) 0.0625(13) 0.017(2) Uani 1 1 d . B 1 C19 C 0.1707(5) 0.1937(5) 1.0634(14) 0.022(2) Uani 1 1 d . A 1 C14 C 0.4193(6) 0.3429(6) 0.8120(16) 0.029(3) Uani 1 1 d . A 1 H14 H 0.4037 0.3264 0.9242 0.035 Uiso 1 1 calc R A 1 C3 C 0.4712(6) 0.1406(6) -0.1007(15) 0.028(3) Uani 1 1 d . B 1 H3 H 0.4893 0.1845 -0.1598 0.033 Uiso 1 1 calc R B 1 C18 C 0.1950(6) 0.1934(6) 0.8954(15) 0.026(3) Uani 1 1 d . A 1 H18 H 0.1760 0.1499 0.8340 0.032 Uiso 1 1 calc R A 1 F4 F 0.3354(5) 0.4832(4) 1.0122(15) 0.086(4) Uani 1 1 d . A 1 C25 C -0.2591(6) -0.1983(6) 1.1469(15) 0.031(3) Uani 1 1 d . C 1 H25 H -0.2599 -0.1816 1.0358 0.037 Uiso 1 1 calc R C 1 C29 C -0.1926(6) -0.1948(6) 1.4013(14) 0.025(2) Uani 1 1 d . C 1 H29 H -0.1490 -0.1760 1.4622 0.030 Uiso 1 1 calc R C 1 C7 C 0.4693(6) 0.0756(6) 0.1518(16) 0.030(3) Uani 1 1 d . B 1 H7 H 0.4856 0.0753 0.2634 0.036 Uiso 1 1 calc R B 1 F1 F 0.2615(4) 0.3665(5) 0.5571(12) 0.058(2) Uani 1 1 d . A 1 C20 C 0.1995(6) 0.2597(6) 1.1515(16) 0.030(3) Uani 1 1 d . A 1 H20 H 0.1839 0.2606 1.2637 0.036 Uiso 1 1 calc R A 1 C13 C 0.4721(6) 0.3310(5) 0.7316(16) 0.028(3) Uani 1 1 d . A 1 H13 H 0.4910 0.3059 0.7903 0.034 Uiso 1 1 calc R A 1 F3 F 0.3313(5) 0.4808(4) 0.6198(14) 0.080(3) Uani 1 1 d . A 1 C27 C -0.3234(6) -0.2765(6) 1.3868(15) 0.025(3) Uani 1 1 d . C 1 C17 C 0.2473(6) 0.2576(6) 0.8196(17) 0.031(3) Uani 1 1 d . A 1 H17 H 0.2636 0.2570 0.7080 0.037 Uiso 1 1 calc R A 1 C4 C 0.4188(6) 0.0767(6) -0.1801(15) 0.029(3) Uani 1 1 d . B 1 H4 H 0.4028 0.0780 -0.2916 0.035 Uiso 1 1 calc R B 1 F10 F -0.3666(5) -0.2614(4) 1.7408(13) 0.059(2) Uani 1 1 d . D 1 C16 C 0.2757(6) 0.3232(6) 0.9099(17) 0.032(3) Uani 1 1 d . A 1 C6 C 0.4170(6) 0.0106(6) 0.0754(17) 0.035(3) Uani 1 1 d . B 1 H6 H 0.3999 -0.0329 0.1357 0.042 Uiso 1 1 calc R B 1 F5 F 0.4057(4) 0.4391(4) 1.0749(13) 0.062(2) Uani 1 1 d . A 1 C30 C -0.3929(6) -0.3334(6) 1.4838(17) 0.036(3) Uani 1 1 d . . 1 C28 C -0.2580(7) -0.2478(6) 1.4779(16) 0.033(3) Uani 1 1 d . C 1 H28 H -0.2576 -0.2638 1.5900 0.040 Uiso 1 1 calc R C 1 C15 C 0.3329(7) 0.3942(6) 0.8137(18) 0.040(3) Uani 1 1 d . A 1 F9 F -0.4829(4) -0.3358(4) 1.2851(14) 0.076(3) Uani 1 1 d . E 1 F11 F -0.4804(4) -0.3308(5) 1.6781(14) 0.077(3) Uani 1 1 d . D 1 C10 C 0.4682(6) 0.3942(6) 0.4802(16) 0.031(3) Uani 1 1 d . A 1 H10 H 0.4850 0.4119 0.3693 0.038 Uiso 1 1 calc R A 1 F8 F -0.4386(4) -0.4052(4) 1.2238(13) 0.061(2) Uani 1 1 d . E 1 C11 C 0.4169(6) 0.4060(6) 0.5538(17) 0.034(3) Uani 1 1 d . A 1 H11 H 0.3991 0.4316 0.4929 0.041 Uiso 1 1 calc R A 1 F6 F 0.4322(4) 0.5136(4) 0.8623(14) 0.080(3) Uani 1 1 d . A 1 C26 C -0.3243(6) -0.2506(6) 1.2214(16) 0.032(3) Uani 1 1 d . C 1 H26 H -0.3679 -0.2680 1.1614 0.038 Uiso 1 1 calc R C 1 C31 C -0.4575(7) -0.3764(8) 1.352(2) 0.057(5) Uani 1 1 d . E 1 F7 F -0.5136(4) -0.4322(4) 1.4363(14) 0.077(3) Uani 1 1 d . E 1 C21 C 0.2504(6) 0.3231(6) 1.0748(16) 0.033(3) Uani 1 1 d . A 1 H21 H 0.2681 0.3667 1.1347 0.039 Uiso 1 1 calc R A 1 F2 F 0.2339(4) 0.4142(4) 0.7677(15) 0.082(4) Uani 1 1 d . A 1 C32 C -0.4143(9) -0.2907(8) 1.610(2) 0.057(5) Uani 1 1 d . D 1 C12 C 0.3906(6) 0.3801(5) 0.7200(17) 0.029(3) Uani 1 1 d . A 1 C5 C 0.3900(6) 0.0100(6) -0.0903(16) 0.028(3) Uani 1 1 d . B 1 C33 C 0.2889(8) 0.4126(8) 0.684(2) 0.055(5) Uani 1 1 d . A 1 F12 F -0.4145(4) -0.2338(4) 1.5303(14) 0.076(3) Uani 1 1 d . D 1 C34 C 0.3772(8) 0.4576(7) 0.946(2) 0.054(4) Uani 1 1 d . A 1 C100 C 0.3268 0.6480 0.6206 0.094 Uiso 0.25 1 d P F 1 C101 C 0.3496 0.7055 0.4859 0.140 Uiso 0.25 1 d P . 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 O5 0.034(5) 0.026(4) 0.033(5) 0.015(4) 0.016(4) 0.012(4) O4 0.034(5) 0.026(4) 0.032(5) -0.016(4) -0.018(4) 0.016(4) Zn1 0.0112(6) 0.0111(6) 0.0190(6) 0.0018(5) 0.0014(5) 0.0016(5) Zn2 0.0109(6) 0.0120(6) 0.0193(6) -0.0015(5) -0.0012(5) 0.0026(5) C1 0.025(6) 0.029(7) 0.039(8) -0.017(6) -0.008(5) 0.022(6) C23 0.021(6) 0.023(6) 0.041(8) 0.005(5) 0.013(6) 0.015(5) C8 0.018(6) 0.021(6) 0.041(8) -0.015(5) -0.005(5) 0.011(5) O8 0.020(4) 0.021(4) 0.029(5) 0.008(3) 0.011(3) 0.004(3) C22 0.013(5) 0.013(6) 0.045(8) 0.021(5) 0.004(5) 0.006(5) O2 0.043(5) 0.032(5) 0.035(5) -0.002(4) 0.013(4) 0.025(4) O3 0.023(4) 0.035(5) 0.036(5) -0.002(4) 0.003(3) 0.022(4) O7 0.012(4) 0.016(4) 0.040(5) 0.003(3) 0.008(3) -0.001(3) O1 0.015(4) 0.013(4) 0.043(5) -0.003(3) -0.007(3) -0.002(3) O6 0.029(4) 0.026(4) 0.029(5) 0.010(3) 0.015(4) 0.011(4) C9 0.011(5) 0.017(5) 0.033(6) 0.002(5) 0.011(4) 0.005(4) C24 0.008(5) 0.006(5) 0.038(7) 0.010(4) 0.006(4) -0.002(4) C2 0.006(5) 0.005(5) 0.033(6) -0.001(4) -0.006(4) -0.001(4) C19 0.016(5) 0.016(5) 0.035(7) 0.000(5) 0.006(5) 0.008(5) C14 0.015(6) 0.021(6) 0.048(8) 0.007(5) 0.015(5) 0.007(5) C3 0.027(6) 0.021(6) 0.038(7) 0.002(5) -0.007(5) 0.015(5) C18 0.021(6) 0.024(6) 0.046(7) 0.005(5) 0.010(5) 0.020(5) F4 0.070(6) 0.015(4) 0.168(10) 0.000(5) 0.073(6) 0.017(4) C25 0.033(7) 0.017(6) 0.038(7) 0.020(5) 0.014(5) 0.009(5) C29 0.017(5) 0.023(6) 0.039(7) 0.002(5) 0.003(5) 0.015(5) C7 0.014(6) 0.027(6) 0.045(8) -0.014(5) -0.016(5) 0.006(5) F1 0.035(5) 0.051(6) 0.094(7) 0.027(5) 0.010(4) 0.026(4) C20 0.023(6) 0.025(6) 0.042(8) 0.006(5) 0.013(5) 0.012(5) C13 0.025(6) 0.008(5) 0.054(8) 0.006(5) 0.010(5) 0.010(5) F3 0.058(6) 0.039(5) 0.166(10) 0.063(6) 0.065(6) 0.041(5) C27 0.021(6) 0.022(6) 0.040(7) 0.015(5) 0.006(5) 0.017(5) C17 0.024(6) 0.020(6) 0.053(8) 0.008(5) 0.016(5) 0.015(5) C4 0.019(6) 0.034(7) 0.034(7) -0.007(5) -0.019(5) 0.013(5) F10 0.057(6) 0.039(5) 0.090(7) 0.013(5) 0.032(5) 0.030(5) C16 0.017(6) 0.024(6) 0.057(8) 0.024(6) 0.023(5) 0.010(5) C6 0.021(6) 0.014(6) 0.061(9) 0.004(5) -0.015(6) 0.002(5) F5 0.036(5) 0.039(5) 0.098(7) -0.027(5) 0.016(5) 0.008(4) C30 0.021(6) 0.024(6) 0.067(9) 0.023(6) 0.013(6) 0.013(5) C28 0.044(8) 0.033(7) 0.032(7) 0.023(5) 0.014(6) 0.027(6) C15 0.030(7) 0.020(6) 0.070(9) 0.014(6) 0.039(6) 0.013(6) F9 0.017(4) 0.050(5) 0.158(9) 0.051(6) -0.008(5) 0.015(4) F11 0.044(5) 0.053(6) 0.153(9) 0.058(6) 0.064(6) 0.039(5) C10 0.015(6) 0.027(7) 0.056(8) 0.010(5) 0.019(5) 0.013(5) F8 0.035(5) 0.041(5) 0.092(7) 0.020(5) -0.027(5) 0.008(4) C11 0.026(6) 0.018(6) 0.063(9) 0.023(6) 0.026(6) 0.016(5) F6 0.047(5) 0.012(4) 0.159(9) 0.007(5) 0.069(6) -0.002(4) C26 0.020(6) 0.033(7) 0.047(8) 0.018(6) 0.006(5) 0.016(5) C31 0.029(8) 0.039(8) 0.096(13) 0.057(9) 0.005(8) 0.013(7) F7 0.015(4) 0.041(5) 0.162(9) 0.065(6) 0.005(5) 0.003(4) C21 0.025(6) 0.007(5) 0.057(8) 0.000(5) 0.029(6) 0.002(5) F2 0.048(5) 0.060(6) 0.168(10) 0.069(6) 0.069(6) 0.050(5) C32 0.054(10) 0.029(8) 0.105(14) 0.046(9) 0.050(10) 0.033(8) C12 0.021(6) 0.005(5) 0.065(9) 0.011(5) 0.016(6) 0.008(5) C5 0.024(6) 0.013(5) 0.054(8) -0.011(5) -0.025(5) 0.015(5) C33 0.039(8) 0.036(8) 0.112(14) 0.048(9) 0.049(9) 0.035(7) F12 0.053(5) 0.047(5) 0.159(9) 0.064(5) 0.063(5) 0.048(5) C34 0.037(8) 0.026(7) 0.093(13) 0.008(8) 0.048(9) 0.011(6) _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 O5 C22 1.259(14) . ? O5 Zn2 1.928(7) 2 ? O4 C1 1.243(14) . ? O4 Zn1 1.925(7) 2_655 ? Zn1 O1 1.926(7) . ? Zn1 O4 1.925(7) 3_664 ? Zn1 O2 1.934(8) . ? Zn1 O3 1.941(7) 3_664 ? Zn2 O7 1.923(7) . ? Zn2 O5 1.928(7) 3_554 ? Zn2 O8 1.935(7) . ? Zn2 O6 1.938(7) 2 ? C1 O1 1.265(14) . ? C1 C2 1.528(14) . ? C23 O6 1.246(14) . ? C23 O8 1.269(14) . ? C23 C24 1.506(14) . ? C8 O2 1.243(14) . ? C8 O3 1.252(13) . ? C8 C9 1.524(15) . ? C22 O7 1.277(13) . ? C22 C19 1.510(14) . ? O3 Zn1 1.941(7) 2_655 ? O6 Zn2 1.938(7) 3_554 ? C9 C10 1.375(15) . ? C9 C13 1.380(15) . ? C24 C25 1.384(15) . ? C24 C29 1.401(15) . ? C2 C7 1.374(15) . ? C2 C3 1.371(14) . ? C19 C20 1.393(15) . ? C19 C18 1.396(15) . ? C14 C12 1.407(15) . ? C14 C13 1.410(15) . ? C3 C4 1.394(15) . ? C18 C17 1.385(15) . ? F4 C34 1.350(15) . ? C25 C26 1.393(15) . ? C29 C28 1.407(15) . ? C7 C6 1.396(15) . ? F1 C33 1.296(19) . ? C20 C21 1.369(15) . ? F3 C33 1.360(14) . ? C27 C26 1.392(15) . ? C27 C28 1.394(16) . ? C27 C30 1.553(15) . ? C17 C16 1.396(17) . ? C4 C5 1.411(16) . ? F10 C32 1.341(19) . ? C16 C21 1.380(16) . ? C16 C15 1.570(15) . ? C6 C5 1.397(16) . ? F5 C34 1.320(18) . ? C30 C5 1.535(15) 3_556 ? C30 C32 1.55(2) . ? C30 C31 1.58(2) . ? C15 C33 1.55(2) . ? C15 C34 1.57(2) . ? C15 C12 1.575(15) . ? F9 C31 1.328(14) . ? F11 C32 1.331(15) . ? C10 C11 1.358(15) . ? F8 C31 1.327(19) . ? C11 C12 1.396(16) . ? F6 C34 1.344(14) . ? C31 F7 1.353(14) . ? F2 C33 1.349(14) . ? C32 F12 1.357(14) . ? C5 C30 1.535(15) 2_553 ? C100 C101 1.4868 . ? C100 C101 1.6636 2_665 ? C101 C100 1.6636 3_564 ? 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 C22 O5 Zn2 136.3(7) . 2 ? C1 O4 Zn1 136.2(8) . 2_655 ? O1 Zn1 O4 104.0(3) . 3_664 ? O1 Zn1 O2 101.9(3) . . ? O4 Zn1 O2 105.2(3) 3_664 . ? O1 Zn1 O3 136.1(3) . 3_664 ? O4 Zn1 O3 102.2(3) 3_664 3_664 ? O2 Zn1 O3 104.3(3) . 3_664 ? O7 Zn2 O5 104.6(3) . 3_554 ? O7 Zn2 O8 136.0(3) . . ? O5 Zn2 O8 102.1(3) 3_554 . ? O7 Zn2 O6 102.4(3) . 2 ? O5 Zn2 O6 104.3(3) 3_554 2 ? O8 Zn2 O6 104.1(3) . 2 ? O4 C1 O1 126.9(11) . . ? O4 C1 C2 117.3(11) . . ? O1 C1 C2 115.7(10) . . ? O6 C23 O8 126.6(10) . . ? O6 C23 C24 116.9(10) . . ? O8 C23 C24 116.3(10) . . ? O2 C8 O3 127.1(10) . . ? O2 C8 C9 116.1(10) . . ? O3 C8 C9 116.8(11) . . ? C23 O8 Zn2 128.9(7) . . ? O5 C22 O7 125.4(9) . . ? O5 C22 C19 117.6(10) . . ? O7 C22 C19 116.9(10) . . ? C8 O2 Zn1 136.6(8) . . ? C8 O3 Zn1 128.8(7) . 2_655 ? C22 O7 Zn2 130.1(7) . . ? C1 O1 Zn1 129.0(7) . . ? C23 O6 Zn2 135.9(8) . 3_554 ? C10 C9 C13 119.7(10) . . ? C10 C9 C8 120.1(10) . . ? C13 C9 C8 120.2(10) . . ? C25 C24 C29 118.8(9) . . ? C25 C24 C23 119.5(10) . . ? C29 C24 C23 121.8(10) . . ? C7 C2 C3 119.7(9) . . ? C7 C2 C1 117.7(9) . . ? C3 C2 C1 122.5(9) . . ? C20 C19 C18 118.7(10) . . ? C20 C19 C22 119.0(10) . . ? C18 C19 C22 122.3(10) . . ? C12 C14 C13 119.0(11) . . ? C2 C3 C4 121.4(10) . . ? C17 C18 C19 120.2(11) . . ? C24 C25 C26 122.1(10) . . ? C24 C29 C28 119.7(10) . . ? C2 C7 C6 120.3(11) . . ? C21 C20 C19 120.8(11) . . ? C9 C13 C14 120.3(10) . . ? C26 C27 C28 119.7(10) . . ? C26 C27 C30 123.6(10) . . ? C28 C27 C30 116.6(10) . . ? C18 C17 C16 120.3(11) . . ? C3 C4 C5 119.7(10) . . ? C21 C16 C17 119.0(10) . . ? C21 C16 C15 123.4(11) . . ? C17 C16 C15 117.6(11) . . ? C5 C6 C7 121.0(11) . . ? C5 C30 C32 112.7(11) 3_556 . ? C5 C30 C27 111.2(9) 3_556 . ? C32 C30 C27 106.9(9) . . ? C5 C30 C31 106.8(10) 3_556 . ? C32 C30 C31 108.6(12) . . ? C27 C30 C31 110.7(10) . . ? C27 C28 C29 120.4(10) . . ? C33 C15 C16 105.9(10) . . ? C33 C15 C34 112.5(12) . . ? C16 C15 C34 111.0(11) . . ? C33 C15 C12 112.1(11) . . ? C16 C15 C12 109.6(9) . . ? C34 C15 C12 105.7(10) . . ? C11 C10 C9 121.4(11) . . ? C10 C11 C12 120.7(11) . . ? C27 C26 C25 119.3(11) . . ? F9 C31 F8 108.8(13) . . ? F9 C31 F7 106.9(10) . . ? F8 C31 F7 106.9(13) . . ? F9 C31 C30 113.1(13) . . ? F8 C31 C30 111.7(11) . . ? F7 C31 C30 109.1(12) . . ? C20 C21 C16 121.0(11) . . ? F11 C32 F10 108.1(14) . . ? F11 C32 F12 106.2(10) . . ? F10 C32 F12 105.4(13) . . ? F11 C32 C30 113.4(13) . . ? F10 C32 C30 111.7(11) . . ? F12 C32 C30 111.6(13) . . ? C11 C12 C14 118.9(10) . . ? C11 C12 C15 122.8(10) . . ? C14 C12 C15 118.2(11) . . ? C6 C5 C4 117.9(9) . . ? C6 C5 C30 123.7(10) . 2_553 ? C4 C5 C30 118.3(10) . 2_553 ? F1 C33 F2 108.3(13) . . ? F1 C33 F3 109.8(14) . . ? F2 C33 F3 105.5(10) . . ? F1 C33 C15 113.4(10) . . ? F2 C33 C15 109.6(13) . . ? F3 C33 C15 110.0(13) . . ? F5 C34 F6 107.5(13) . . ? F5 C34 F4 109.0(14) . . ? F6 C34 F4 106.2(10) . . ? F5 C34 C15 113.7(11) . . ? F6 C34 C15 109.2(12) . . ? F4 C34 C15 110.9(13) . . ? C101 C100 C101 129.9 . 2_665 ? C100 C101 C100 113.7 . 3_564 ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.958 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.137