# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: modulation of size and shape of cuboid 3-D coordination networks ; loop_ _publ_author_name 'Mir Wais Hosseini' 'Abdelaziz Jouaiti' 'Nathalie Kyritsakas' 'Mei-Jin Lin.' # Attachment 'New 1-ZnSiF6.cif' data_e1267a _database_code_depnum_ccdc_archive 'CCDC 693608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C20 H16 F6 N4 Si Zn), 36(H2 O)' _chemical_formula_sum 'C80 H136 F24 N16 O36 Si4 Zn4' _chemical_formula_weight 2727.89 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' 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' O O 0.0106 0.0060 '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 Tetragonal _symmetry_space_group_name_H-M I4/mcm _symmetry_space_group_name_Hall '-I 4 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 16.0491(8) _cell_length_b 16.0491(8) _cell_length_c 15.3683(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3958.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 643 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.83 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9188 _exptl_absorpt_correction_T_max 0.9582 _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 6674 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1229 _reflns_number_gt 881 _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^)+(0.1974P)^2^+31.3990P] 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 1229 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.3060 _refine_ls_wR_factor_gt 0.2779 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.0000 1.0000 0.2500 0.0101(5) Uani 1 8 d S . . Si2 Si 0.0000 1.0000 0.0000 0.0151(8) Uani 1 8 d S . . F1 F 0.0000 1.0000 0.1119(4) 0.0242(14) Uani 1 4 d S A . F2 F -0.0220(6) 1.1015(4) 0.0000 0.040 Uani 0.684(10) 2 d SP A 1 F3 F 0.0305(14) 1.0971(9) 0.0000 0.040 Uani 0.316(10) 2 d SP A 2 N1 N 0.0939(2) 0.9061(2) 0.2500 0.0195(13) Uani 1 2 d S . . C1 C 0.0987(5) 0.8499(4) 0.3130(5) 0.0506(19) Uani 1 1 d . . . H1 H 0.0591 0.8522 0.3589 0.061 Uiso 1 1 calc R . . C2 C 0.1585(5) 0.7883(5) 0.3147(5) 0.055(2) Uani 1 1 d . . . H2 H 0.1592 0.7493 0.3611 0.066 Uiso 1 1 calc R . . C3 C 0.2170(3) 0.7830(3) 0.2500 0.0285(17) Uani 1 2 d S . . O1 O 0.2485(17) 0.7956(13) 0.5000 0.093(6) Uani 0.50 2 d SP . . O2 O 0.3498(10) 0.8498(10) 0.0000 0.063(6) Uani 0.50 4 d SP . . O3 O 0.2895(7) 0.0585(8) 0.0943(9) 0.075(3) Uani 0.50 1 d P . . O4 O 0.264(2) 0.978(3) 0.0000 0.073(9) Uani 0.25 2 d SP . . O5 O 0.411(5) 0.0000 0.2500 0.15(3) Uani 0.25 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 0.0084(6) 0.0084(6) 0.0135(8) 0.000 0.000 0.000 Si2 0.0167(11) 0.0167(11) 0.0119(17) 0.000 0.000 0.000 F1 0.030(2) 0.030(2) 0.013(3) 0.000 0.000 0.000 F2 0.072 0.022 0.025 0.000 0.000 0.024 F3 0.072 0.022 0.025 0.000 0.000 0.024 N1 0.0130(17) 0.0130(17) 0.033(3) 0.0009(16) 0.0009(16) 0.007(2) C1 0.052(4) 0.048(4) 0.052(4) 0.025(3) 0.023(3) 0.034(3) C2 0.056(4) 0.052(4) 0.058(4) 0.029(3) 0.027(3) 0.038(4) C3 0.021(2) 0.021(2) 0.044(5) 0.003(2) 0.003(2) 0.009(3) O1 0.144(17) 0.091(13) 0.043(9) 0.000 0.000 0.048(12) O2 0.076(9) 0.076(9) 0.036(11) 0.000 0.000 -0.006(12) O3 0.067(8) 0.071(8) 0.087(8) 0.012(7) -0.011(6) -0.018(6) O4 0.05(2) 0.10(2) 0.06(2) 0.000 0.000 -0.004(19) O5 0.21(7) 0.18(6) 0.05(2) -0.05(3) 0.000 0.000 _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 2.122(6) . ? Zn1 F1 2.122(6) 5 ? Zn1 N1 2.132(6) . ? Zn1 N1 2.132(6) 3_665 ? Zn1 N1 2.132(6) 4_465 ? Zn1 N1 2.132(6) 2_575 ? Si2 F3 1.633(16) 17_575 ? Si2 F3 1.633(16) . ? Si2 F3 1.633(16) 19_465 ? Si2 F3 1.633(16) 3_665 ? Si2 F2 1.666(7) 19_465 ? Si2 F2 1.666(7) 17_575 ? Si2 F2 1.666(7) . ? Si2 F2 1.666(7) 3_665 ? Si2 F1 1.720(6) 17_575 ? Si2 F1 1.720(6) . ? N1 C1 1.324(7) 8_665 ? N1 C1 1.324(7) . ? C1 C2 1.378(8) . ? C1 H1 0.9500 . ? C2 C3 1.370(7) . ? C2 H2 0.9500 . ? C3 C2 1.370(7) 8_665 ? C3 C3 1.497(15) 25_565 ? 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) . 5 ? F1 Zn1 N1 90.0 . . ? F1 Zn1 N1 90.0 5 . ? F1 Zn1 N1 90.000(1) . 3_665 ? F1 Zn1 N1 90.001(1) 5 3_665 ? N1 Zn1 N1 90.0 . 3_665 ? F1 Zn1 N1 90.000(1) . 4_465 ? F1 Zn1 N1 89.999(1) 5 4_465 ? N1 Zn1 N1 90.0 . 4_465 ? N1 Zn1 N1 180.0 3_665 4_465 ? F1 Zn1 N1 90.0 . 2_575 ? F1 Zn1 N1 90.0 5 2_575 ? N1 Zn1 N1 180.00(15) . 2_575 ? N1 Zn1 N1 90.000(1) 3_665 2_575 ? N1 Zn1 N1 90.0 4_465 2_575 ? F3 Si2 F3 179.997(3) 17_575 . ? F3 Si2 F3 90.002(2) 17_575 19_465 ? F3 Si2 F3 90.001(2) . 19_465 ? F3 Si2 F3 89.997(2) 17_575 3_665 ? F3 Si2 F3 90.000(2) . 3_665 ? F3 Si2 F3 179.999(2) 19_465 3_665 ? F3 Si2 F2 119.7(7) 17_575 19_465 ? F3 Si2 F2 60.3(7) . 19_465 ? F3 Si2 F2 150.3(7) 3_665 19_465 ? F2 Si2 F2 90.002(2) 19_465 17_575 ? F3 Si2 F2 150.3(7) 17_575 . ? F3 Si2 F2 119.7(7) 19_465 . ? F3 Si2 F2 60.3(7) 3_665 . ? F2 Si2 F2 90.001(1) 19_465 . ? F2 Si2 F2 179.997(2) 17_575 . ? F3 Si2 F2 60.3(7) 17_575 3_665 ? F3 Si2 F2 119.7(7) . 3_665 ? F3 Si2 F2 150.3(7) 19_465 3_665 ? F2 Si2 F2 180.0 19_465 3_665 ? F2 Si2 F2 89.999(1) 17_575 3_665 ? F2 Si2 F2 89.998(1) . 3_665 ? F3 Si2 F1 90.0 17_575 17_575 ? F3 Si2 F1 90.0 . 17_575 ? F3 Si2 F1 90.001(1) 19_465 17_575 ? F3 Si2 F1 89.999(1) 3_665 17_575 ? F2 Si2 F1 90.001(1) 19_465 17_575 ? F2 Si2 F1 90.0 17_575 17_575 ? F2 Si2 F1 90.0 . 17_575 ? F2 Si2 F1 89.999(1) 3_665 17_575 ? F3 Si2 F1 90.0 17_575 . ? F3 Si2 F1 90.0 . . ? F3 Si2 F1 90.000(1) 19_465 . ? F3 Si2 F1 90.000(1) 3_665 . ? F2 Si2 F1 90.000(1) 19_465 . ? F2 Si2 F1 90.0 17_575 . ? F2 Si2 F1 90.0 . . ? F2 Si2 F1 90.000(1) 3_665 . ? F1 Si2 F1 179.999(1) 17_575 . ? Si2 F1 Zn1 180.0 . . ? C1 N1 C1 117.1(7) 8_665 . ? C1 N1 Zn1 121.4(3) 8_665 . ? C1 N1 Zn1 121.4(3) . . ? N1 C1 C2 122.8(6) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 120.6(6) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C2 116.1(7) . 8_665 ? C2 C3 C3 122.0(4) . 25_565 ? C2 C3 C3 122.0(4) 8_665 25_565 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.388 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.251 # Attachment 'New 2-ZnSiF6.cif' data_e1268a _database_code_depnum_ccdc_archive 'CCDC 693609' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 F6 N4 Si Zn, 0.242(C4 H4 Cl12), C2 H2 Cl6' _chemical_formula_sum 'C26.97 H18.97 Cl8.90 F6 N4 Si Zn' _chemical_formula_weight 922.17 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' Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/mcm _symmetry_space_group_name_Hall '-I 4 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 19.5940(3) _cell_length_b 19.5940(3) _cell_length_c 15.0666(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5784.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2277 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 23.83 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832.6 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8999 _exptl_absorpt_correction_T_max 0.9398 _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 22910 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.59 _reflns_number_total 1813 _reflns_number_gt 1421 _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^)+(0.1741P)^2^+35.8575P] 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 1813 _refine_ls_number_parameters 81 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1601 _refine_ls_R_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.3287 _refine_ls_wR_factor_gt 0.2958 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.035 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 1.0000 1.0000 0.7500 0.0292(6) Uani 1 8 d S . . Si1 Si 1.0000 1.0000 1.0000 0.0360(10) Uani 1 8 d S . . F1 F 1.0000 1.0000 0.8873(4) 0.051(2) Uani 1 4 d S . . F2 F 1.0831(3) 0.9816(3) 1.0000 0.0504(15) Uani 1 2 d S . . N1 N 0.9233(3) 0.9233(3) 0.7500 0.0428(17) Uani 1 2 d S . . C1 C 0.9212(4) 0.8762(3) 0.6858(4) 0.0446(16) Uani 1 1 d . . . H1 H 0.9545 0.8776 0.6400 0.054 Uiso 1 1 calc R . . C2 C 0.8721(4) 0.8255(4) 0.6839(5) 0.0557(19) Uani 1 1 d . . . H2 H 0.8720 0.7925 0.6377 0.067 Uiso 1 1 calc R . . C3 C 0.8233(4) 0.8233(4) 0.7500 0.058(3) Uani 1 2 d S . . C4 C 0.7709(4) 0.7709(4) 0.7500 0.069(3) Uani 1 2 d S . . C5 C 0.9139(18) 0.2250(13) 0.5000 0.080(8) Uani 0.50 2 d SP . . H5 H 0.9169 0.1741 0.5000 0.096 Uiso 0.50 2 calc SPR . . Cl1 Cl 0.9579(5) 0.2509(5) 0.4065(7) 0.133(3) Uani 0.50 1 d P . . Cl2 Cl 0.8360(7) 0.2414(7) 0.5000 0.142(5) Uani 0.50 2 d SP . . C6 C 0.868(3) 0.595(6) 0.555(5) 0.210 Uani 0.121(3) 1 d PD . . H6 H 0.8407 0.5518 0.5579 0.252 Uiso 0.121(3) 1 calc PR . . Cl3 Cl 0.9491(15) 0.5822(15) 0.512(8) 0.210 Uani 0.121(3) 1 d PD . . Cl5 Cl 0.8194(18) 0.6626(17) 0.510(12) 0.210 Uani 0.121(3) 1 d PD . . Cl4 Cl 0.880(4) 0.630(4) 0.660(4) 0.210 Uani 0.121(3) 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 Zn1 0.0353(7) 0.0353(7) 0.0171(8) 0.000 0.000 0.000 Si1 0.0469(16) 0.0469(16) 0.0144(18) 0.000 0.000 0.000 F1 0.069(3) 0.069(3) 0.014(3) 0.000 0.000 0.000 F2 0.043(3) 0.075(4) 0.033(3) 0.000 0.000 0.010(3) N1 0.047(3) 0.047(3) 0.034(4) -0.004(3) 0.004(3) -0.004(3) C1 0.060(4) 0.040(3) 0.033(3) -0.005(3) 0.011(3) -0.009(3) C2 0.072(5) 0.050(4) 0.045(4) -0.010(3) 0.002(4) -0.016(4) C3 0.058(4) 0.058(4) 0.059(6) 0.011(4) -0.011(4) -0.021(5) C4 0.067(4) 0.067(4) 0.073(8) 0.007(5) -0.007(5) -0.019(5) C5 0.12(2) 0.038(12) 0.085(19) 0.000 0.000 0.010(13) Cl1 0.134(7) 0.114(5) 0.152(7) -0.020(5) 0.028(6) -0.002(5) Cl2 0.162(11) 0.171(11) 0.094(7) 0.000 0.000 0.077(9) C6 0.133 0.133 0.363 0.000 0.026 0.025 Cl3 0.133 0.133 0.363 0.000 0.026 0.025 Cl5 0.133 0.133 0.363 0.000 0.026 0.025 Cl4 0.133 0.133 0.363 0.000 0.026 0.025 _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 2.069(7) . ? Zn1 F1 2.069(7) 5_756 ? Zn1 N1 2.124(8) . ? Zn1 N1 2.124(8) 3_755 ? Zn1 N1 2.124(8) 2_775 ? Zn1 N1 2.124(8) 4_575 ? Si1 F2 1.668(6) 17_777 ? Si1 F2 1.668(6) 19_577 ? Si1 F2 1.668(6) . ? Si1 F2 1.668(6) 3_755 ? Si1 F1 1.698(7) 17_777 ? Si1 F1 1.698(7) . ? N1 C1 1.339(7) . ? N1 C1 1.339(7) 7_556 ? C1 C2 1.383(10) . ? C1 H1 0.9500 . ? C2 C3 1.382(10) . ? C2 H2 0.9500 . ? C3 C2 1.382(10) 7_556 ? C3 C4 1.452(15) . ? C4 C4 1.16(2) 25_666 ? C5 Cl2 1.56(4) . ? C5 Cl1 1.73(2) . ? C5 Cl1 1.73(2) 18_556 ? C5 H5 1.0000 . ? C6 Cl4 1.74(2) . ? C6 Cl3 1.74(2) . ? C6 Cl5 1.76(3) . ? C6 H6 1.0000 . ? 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 179.998(1) . 5_756 ? N1 Zn1 N1 179.999(1) . 2_775 ? N1 Zn1 N1 90.000(1) 3_755 2_775 ? F1 Zn1 N1 90.000(1) . 4_575 ? F1 Zn1 N1 89.999(1) 5_756 4_575 ? N1 Zn1 N1 90.001(1) . 4_575 ? N1 Zn1 N1 179.997(1) 3_755 4_575 ? N1 Zn1 N1 89.997(1) 2_775 4_575 ? F2 Si1 F2 90.003(2) 17_777 19_577 ? F2 Si1 F2 179.999(1) 17_777 . ? F2 Si1 F2 89.998(1) 19_577 . ? F2 Si1 F2 89.996(1) 17_777 3_755 ? F2 Si1 F2 180.00(8) 19_577 3_755 ? F2 Si1 F2 90.003(2) . 3_755 ? Si1 F1 Zn1 180.0 . . ? C1 N1 C1 118.6(8) . 7_556 ? C1 N1 Zn1 120.7(4) . . ? C1 N1 Zn1 120.7(4) 7_556 . ? N1 C1 C2 122.2(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.3(7) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C2 118.5(10) . 7_556 ? C2 C3 C4 120.8(5) . . ? C2 C3 C4 120.7(5) 7_556 . ? C4 C4 C3 179.964(3) 25_666 . ? Cl2 C5 Cl1 115.3(11) . . ? Cl2 C5 Cl1 115.3(11) . 18_556 ? Cl1 C5 Cl1 109(2) . 18_556 ? Cl2 C5 H5 105.3 . . ? Cl1 C5 H5 105.3 . . ? Cl1 C5 H5 105.3 18_556 . ? Cl4 C6 Cl3 105(6) . . ? Cl4 C6 Cl5 98(9) . . ? Cl3 C6 Cl5 117(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.401 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.260 # Attachment 'New 3-ZnSiF6.cif' data_e1215a _database_code_depnum_ccdc_archive 'CCDC 693610' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 F6 N4 Si Zn' _chemical_formula_sum 'C32 H24 F6 N4 Si Zn' _chemical_formula_weight 672.01 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' 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' 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 Tetragonal _symmetry_space_group_name_H-M I4/mcm _symmetry_space_group_name_Hall '-I 4 2 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1' 'y+1/2, x+1/2, -z+1' '-y+1/2, -x+1/2, -z+1' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 22.0593(13) _cell_length_b 22.0593(13) _cell_length_c 15.0937(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7344.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 730 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 22.17 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 0.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9777 _exptl_absorpt_correction_T_max 0.9850 _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 10236 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2262 _reflns_number_gt 1274 _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^)+(0.0963P)^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 2262 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1927 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.0000 0.0000 0.2500 0.0172(3) Uani 1 8 d S . . Si1 Si 0.0000 0.0000 0.0000 0.0207(5) Uani 1 8 d S . . F1 F 0.01785(16) -0.07277(13) 0.0000 0.0469(9) Uani 1 2 d S . . F2 F 0.0000 0.0000 0.1134(2) 0.0349(9) Uani 1 4 d S . . N1 N 0.06787(10) 0.06787(10) 0.2500 0.0230(7) Uani 1 2 d S . . C1 C 0.06911(16) 0.11100(15) 0.1883(2) 0.0295(8) Uani 1 1 d . . . H1 H 0.0388 0.1103 0.1436 0.035 Uiso 1 1 calc R . . C2 C 0.11251(17) 0.15727(16) 0.1854(3) 0.0378(9) Uani 1 1 d . . . H2 H 0.1113 0.1876 0.1408 0.045 Uiso 1 1 calc R . . C3 C 0.15731(14) 0.15731(14) 0.2500 0.0361(11) Uani 1 2 d S . . C4 C 0.20514(14) 0.20514(14) 0.2500 0.0460(13) Uani 1 2 d S . . C5 C 0.1909(2) 0.2632(2) 0.2295(4) 0.090(2) Uani 1 1 d . . . H5 H 0.1503 0.2735 0.2151 0.108 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 0.0162(3) 0.0162(3) 0.0194(4) 0.000 0.000 0.000 Si1 0.0220(7) 0.0220(7) 0.0181(10) 0.000 0.000 0.000 F1 0.078(3) 0.0244(16) 0.0383(16) 0.000 0.000 0.0143(14) F2 0.0413(13) 0.0413(13) 0.0220(17) 0.000 0.000 0.000 N1 0.0219(10) 0.0219(10) 0.0250(15) -0.0013(14) 0.0013(14) -0.0048(12) C1 0.0289(18) 0.0223(17) 0.0372(17) 0.0033(15) -0.0042(16) -0.0051(13) C2 0.038(2) 0.029(2) 0.047(2) 0.0106(18) -0.0002(18) -0.0082(16) C3 0.0273(14) 0.0273(14) 0.054(3) 0.001(2) -0.001(2) -0.0119(17) C4 0.0342(17) 0.0342(17) 0.070(4) 0.002(3) -0.002(3) -0.016(2) C5 0.036(2) 0.052(3) 0.181(7) 0.045(4) -0.027(3) -0.018(2) _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 F2 2.062(3) 5 ? Zn1 F2 2.062(3) . ? Zn1 N1 2.117(3) . ? Zn1 N1 2.117(3) 2 ? Zn1 N1 2.117(3) 4 ? Zn1 N1 2.117(3) 3 ? Si1 F1 1.653(3) . ? Si1 F1 1.653(3) 19 ? Si1 F1 1.653(3) 3 ? Si1 F1 1.653(3) 17 ? Si1 F2 1.712(3) . ? Si1 F2 1.712(3) 17 ? N1 C1 1.332(4) . ? N1 C1 1.332(4) 7 ? C1 C2 1.400(5) . ? C1 H1 0.9500 . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? C3 C2 1.388(4) 7 ? C3 C4 1.492(6) . ? C4 C5 1.355(5) 7 ? C4 C5 1.355(5) . ? C5 C5 1.432(8) 31 ? C5 H5 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 F2 Zn1 F2 180.0 5 . ? F2 Zn1 N1 90.0 5 . ? F2 Zn1 N1 90.0 . . ? F2 Zn1 N1 90.0 5 2 ? F2 Zn1 N1 90.0 . 2 ? N1 Zn1 N1 180.0 . 2 ? F2 Zn1 N1 90.0 5 4 ? F2 Zn1 N1 90.0 . 4 ? N1 Zn1 N1 90.0 . 4 ? N1 Zn1 N1 90.0 2 4 ? F2 Zn1 N1 90.0 5 3 ? F2 Zn1 N1 90.0 . 3 ? N1 Zn1 N1 90.0 . 3 ? N1 Zn1 N1 90.0 2 3 ? N1 Zn1 N1 180.0 4 3 ? F1 Si1 F1 90.0 . 19 ? F1 Si1 F1 90.0 . 3 ? F1 Si1 F1 180.0 19 3 ? F1 Si1 F1 180.0 . 17 ? F1 Si1 F1 90.0 19 17 ? F1 Si1 F1 90.0 3 17 ? F1 Si1 F2 90.0 . . ? F1 Si1 F2 90.0 19 . ? F1 Si1 F2 90.0 3 . ? F1 Si1 F2 90.0 17 . ? F1 Si1 F2 90.0 . 17 ? F1 Si1 F2 90.0 19 17 ? F1 Si1 F2 90.0 3 17 ? F1 Si1 F2 90.0 17 17 ? F2 Si1 F2 180.0 . 17 ? Si1 F2 Zn1 180.0 . . ? C1 N1 C1 117.4(4) . 7 ? C1 N1 Zn1 121.30(19) . . ? C1 N1 Zn1 121.31(19) 7 . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 117.8(3) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C2 119.5(4) 7 . ? C2 C3 C4 120.3(2) 7 . ? C2 C3 C4 120.3(2) . . ? C5 C4 C5 119.4(5) 7 . ? C5 C4 C3 120.3(2) 7 . ? C5 C4 C3 120.3(2) . . ? C4 C5 C5 120.3(2) . 31 ? C4 C5 H5 119.8 . . ? C5 C5 H5 119.8 31 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.913 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.137