# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'W Levason' 'Fei Cheng' 'Andrew Hector' 'Gillian Reid' 'Michael Webster' 'Wenjian Zhang' _publ_contact_author_name 'W Levason' _publ_contact_author_email WXL@SOTON.AC.UK _publ_section_title ; Preparation and structure of the unique silicon(IV) cation [SiF3(Me3tacn)]+ ; # Attachment 'Si_all3a.cif' data_08wz904 _database_code_depnum_ccdc_archive 'CCDC 713184' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-10-16 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trifluorido(1,4,7-trimethyl-1,4,7-triazacyclononane)silicon(IV) chloride ; # C9H21N3 = Me~3~-tacn = 1,4,7-trimethyl-1,4,7-triazacyclononane # ACD iLab gave (from .skc file) 1,4,7-trimethyl-1,4,7-triazonane # ChemSpider also gave 1,4,7-trimethyl-1,4,7-triazonane & the cyclononane name # SMILES string CN1CCN(C)CCN(C)CC1 # ChemSpider (www.chemspider.com) gave SMILES of N1(CCN(CCN(CC1)C)C)C _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H21 F3 N3 Si 1+, Cl 1-' _chemical_formula_sum 'C9 H21 Cl F3 N3 Si' _chemical_formula_weight 291.83 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _space_group_IT_number 161 _space_group_name_Hall 'R 3 -2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 8.779(2) _cell_length_b 8.779(2) _cell_length_c 29.255(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1952.7(6) _cell_formula_units_Z 6 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2531 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8589 # scaled to Tmax=1, 0.6404 _exptl_absorpt_correction_T_max 1.0000 # 0.7456 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2633 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 27.52 _reflns_number_total 911 _reflns_number_gt 842 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+4.9553P] 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 -0.2(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 911 _refine_ls_number_parameters 53 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _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 Cl1 Cl 0.0000 0.0000 0.96578(5) 0.0212(4) Uani 1 3 d S . . Si1 Si 0.6667 0.3333 0.10668(6) 0.0199(5) Uani 1 3 d S . . N1 N 0.7965(4) 0.5380(4) 0.14952(9) 0.0156(6) Uani 1 1 d . . . F1 F 0.5463(3) 0.1541(3) 0.07762(9) 0.0271(6) Uani 1 1 d . . . C1 C 0.9288(5) 0.7003(5) 0.12527(13) 0.0216(8) Uani 1 1 d . . . H1A H 0.9529 0.8039 0.1434 0.032 Uiso 1 1 calc R . . H1B H 0.8826 0.7066 0.0953 0.032 Uiso 1 1 calc R . . H1C H 1.0378 0.6968 0.1213 0.032 Uiso 1 1 calc R . . C2 C 0.6578(4) 0.5692(5) 0.16940(15) 0.0179(7) Uani 1 1 d . . . H2A H 0.6156 0.6208 0.1460 0.022 Uiso 1 1 calc R . . H2B H 0.7069 0.6528 0.1953 0.022 Uiso 1 1 calc R . . C3 C 0.5062(5) 0.3950(5) 0.18590(13) 0.0185(7) Uani 1 1 d . . . H3A H 0.5398 0.3586 0.2144 0.022 Uiso 1 1 calc R . . H3B H 0.4024 0.4076 0.1924 0.022 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 Cl1 0.0186(6) 0.0186(6) 0.0263(9) 0.000 0.000 0.0093(3) Si1 0.0215(7) 0.0215(7) 0.0169(9) 0.000 0.000 0.0107(4) N1 0.0159(15) 0.0162(15) 0.0125(14) -0.0002(12) -0.0007(12) 0.0064(13) F1 0.0296(12) 0.0271(13) 0.0243(11) -0.0044(10) -0.0010(11) 0.0140(11) C1 0.0213(19) 0.0187(18) 0.0232(19) 0.0038(14) 0.0005(14) 0.0089(16) C2 0.0182(17) 0.0190(18) 0.0195(15) -0.0052(14) -0.0039(12) 0.0114(15) C3 0.0181(18) 0.0194(18) 0.0155(17) -0.0054(14) 0.0008(13) 0.0076(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 F1 1.629(3) 2_655 ? Si1 F1 1.629(3) . ? Si1 F1 1.629(3) 3_665 ? Si1 N1 2.013(3) 3_665 ? Si1 N1 2.013(3) . ? Si1 N1 2.013(3) 2_655 ? N1 C2 1.493(5) . ? N1 C1 1.492(5) . ? N1 C3 1.501(4) 3_665 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.520(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.501(4) 2_655 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? 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 Si1 F1 95.24(15) 2_655 . ? F1 Si1 F1 95.24(15) 2_655 3_665 ? F1 Si1 F1 95.24(15) . 3_665 ? F1 Si1 N1 88.14(12) 2_655 3_665 ? F1 Si1 N1 90.90(12) . 3_665 ? F1 Si1 N1 172.69(17) 3_665 3_665 ? F1 Si1 N1 90.90(12) 2_655 . ? F1 Si1 N1 172.69(17) . . ? F1 Si1 N1 88.14(12) 3_665 . ? N1 Si1 N1 85.32(14) 3_665 . ? F1 Si1 N1 172.69(17) 2_655 2_655 ? F1 Si1 N1 88.14(12) . 2_655 ? F1 Si1 N1 90.90(12) 3_665 2_655 ? N1 Si1 N1 85.32(14) 3_665 2_655 ? N1 Si1 N1 85.32(14) . 2_655 ? C2 N1 C1 109.1(3) . . ? C2 N1 C3 111.5(3) . 3_665 ? C1 N1 C3 108.7(3) . 3_665 ? C2 N1 Si1 104.9(2) . . ? C1 N1 Si1 112.3(2) . . ? C3 N1 Si1 110.4(2) 3_665 . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.9(3) . . ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N1 C3 C2 109.0(3) 2_655 . ? N1 C3 H3A 109.9 2_655 . ? C2 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 2_655 . ? C2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # F1 Si1 N1 C2 -56.1(11) . . . . ? # F1 Si1 N1 C1 -174.4(9) . . . . ? # F1 Si1 N1 C3 64.1(11) . . . 3_665 ? F1 Si1 N1 C2 156.8(2) 2_655 . . . ? F1 Si1 N1 C2 61.6(2) 3_665 . . . ? N1 Si1 N1 C2 -115.15(18) 3_665 . . . ? N1 Si1 N1 C2 -29.5(2) 2_655 . . . ? F1 Si1 N1 C1 38.5(3) 2_655 . . . ? F1 Si1 N1 C1 -56.7(3) 3_665 . . . ? N1 Si1 N1 C1 126.5(3) 3_665 . . . ? N1 Si1 N1 C1 -147.8(3) 2_655 . . . ? F1 Si1 N1 C3 -83.0(2) 2_655 . . 3_665 ? F1 Si1 N1 C3 -178.2(2) 3_665 . . 3_665 ? N1 Si1 N1 C3 5.0(2) 3_665 . . 3_665 ? N1 Si1 N1 C3 90.71(18) 2_655 . . 3_665 ? C1 N1 C2 C3 169.1(3) . . . . ? C3 N1 C2 C3 -70.8(4) 3_665 . . . ? Si1 N1 C2 C3 48.7(3) . . . . ? N1 C2 C3 N1 -46.3(4) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.089 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.105 #===END OF CIF ============================================================== # 08wz802 data_08wz802 _database_code_depnum_ccdc_archive 'CCDC 713185' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-11-05 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrafluorido(1,2-bis(dimethylamino)ethane)silicon(IV) ; # tmeda = 1,2-bis(dimethylamino)ethane # N,N,N',N'-tetramethylethylenediamine # N,N,N',N'-tetramethylethane-1,2-diamine (from iLab naming) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 F4 N2 Si' _chemical_formula_sum 'C6 H16 F4 N2 Si' _chemical_formula_weight 220.30 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.3146(15) _cell_length_b 10.648(2) _cell_length_c 7.6840(15) _cell_angle_alpha 90.00 _cell_angle_beta 112.180(10) _cell_angle_gamma 90.00 _cell_volume 478.40(17) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1109 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 232 _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8945 # 0.9740 _exptl_absorpt_correction_T_max 1.0000 # 0.9817 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5735 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.52 _reflns_number_total 2049 _reflns_number_gt 1960 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.1209P] 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(12) _chemical_absolute_configuration ad _refine_ls_number_reflns 2049 _refine_ls_number_parameters 122 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Si1 Si 0.41114(7) 0.73431(4) 0.23284(6) 0.01472(11) Uani 1 1 d . . . F1 F 0.5905(2) 0.62435(10) 0.35544(16) 0.0192(2) Uani 1 1 d . . . F2 F 0.20136(18) 0.83044(10) 0.11530(15) 0.0196(3) Uani 1 1 d . . . F3 F 0.51176(16) 0.73197(12) 0.06442(13) 0.0226(2) Uani 1 1 d . . . F4 F 0.5762(2) 0.84833(10) 0.35530(17) 0.0231(3) Uani 1 1 d . . . N1 N 0.2002(3) 0.58777(15) 0.1078(2) 0.0165(3) Uani 1 1 d . . . N2 N 0.2650(2) 0.72508(16) 0.42916(17) 0.0158(3) Uani 1 1 d . . . C1 C -0.0071(3) 0.62481(18) -0.0584(3) 0.0226(4) Uani 1 1 d . . . H1A H -0.0916 0.5493 -0.1191 0.034 Uiso 1 1 calc R . . H1B H 0.0398 0.6711 -0.1481 0.034 Uiso 1 1 calc R . . H1C H -0.1054 0.6783 -0.0170 0.034 Uiso 1 1 calc R . . C2 C 0.3189(3) 0.48839(18) 0.0399(3) 0.0227(4) Uani 1 1 d . . . H2A H 0.4588 0.4623 0.1435 0.034 Uiso 1 1 calc R . . H2B H 0.3582 0.5221 -0.0628 0.034 Uiso 1 1 calc R . . H2C H 0.2173 0.4159 -0.0054 0.034 Uiso 1 1 calc R . . C3 C 0.1278(3) 0.53096(18) 0.2541(2) 0.0205(4) Uani 1 1 d . . . H3A H 0.2533 0.4793 0.3416 0.025 Uiso 1 1 calc R . . H3B H -0.0069 0.4761 0.1942 0.025 Uiso 1 1 calc R . . C4 C 0.0685(3) 0.6358(2) 0.3597(3) 0.0218(4) Uani 1 1 d . . . H4A H -0.0703 0.6802 0.2758 0.026 Uiso 1 1 calc R . . H4B H 0.0371 0.6011 0.4671 0.026 Uiso 1 1 calc R . . C5 C 0.1758(4) 0.84869(19) 0.4622(3) 0.0255(4) Uani 1 1 d . . . H5A H 0.0589 0.8788 0.3445 0.038 Uiso 1 1 calc R . . H5B H 0.3015 0.9095 0.5064 0.038 Uiso 1 1 calc R . . H5C H 0.1083 0.8391 0.5572 0.038 Uiso 1 1 calc R . . C6 C 0.4315(3) 0.6816(2) 0.6156(2) 0.0235(4) Uani 1 1 d . . . H6A H 0.3635 0.6911 0.7103 0.035 Uiso 1 1 calc R . . H6B H 0.5712 0.7322 0.6517 0.035 Uiso 1 1 calc R . . H6C H 0.4689 0.5931 0.6070 0.035 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 Si1 0.0148(2) 0.0137(2) 0.0159(2) 0.0005(2) 0.00620(15) -0.0015(2) F1 0.0141(5) 0.0203(6) 0.0228(6) 0.0024(5) 0.0066(4) 0.0014(4) F2 0.0231(6) 0.0147(5) 0.0193(6) 0.0021(4) 0.0060(4) 0.0028(5) F3 0.0266(5) 0.0238(5) 0.0227(5) 0.0000(5) 0.0152(4) -0.0065(6) F4 0.0234(6) 0.0204(6) 0.0247(6) -0.0039(5) 0.0081(5) -0.0098(5) N1 0.0173(8) 0.0145(7) 0.0174(7) 0.0014(6) 0.0062(6) 0.0017(6) N2 0.0156(6) 0.0159(7) 0.0155(6) -0.0009(6) 0.0053(5) -0.0004(7) C1 0.0194(9) 0.0204(9) 0.0215(9) 0.0009(8) 0.0003(7) 0.0000(7) C2 0.0263(10) 0.0166(9) 0.0251(10) -0.0036(7) 0.0096(8) 0.0017(7) C3 0.0212(9) 0.0180(9) 0.0236(9) 0.0010(7) 0.0100(7) -0.0047(7) C4 0.0190(9) 0.0248(10) 0.0242(9) -0.0020(8) 0.0111(8) -0.0073(8) C5 0.0313(11) 0.0223(10) 0.0270(11) -0.0016(8) 0.0157(9) 0.0053(8) C6 0.0248(9) 0.0280(10) 0.0164(9) 0.0021(7) 0.0061(7) -0.0002(8) _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 Si1 F3 1.6432(10) . ? Si1 F4 1.6448(12) . ? Si1 F2 1.6477(11) . ? Si1 F1 1.6541(12) . ? Si1 N1 2.0409(17) . ? Si1 N2 2.0463(14) . ? N1 C3 1.492(2) . ? N1 C1 1.496(2) . ? N1 C2 1.500(2) . ? N2 C5 1.491(3) . ? N2 C4 1.493(2) . ? N2 C6 1.495(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.509(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 F3 Si1 F4 96.42(6) . . ? F3 Si1 F2 92.73(6) . . ? F4 Si1 F2 93.43(7) . . ? F3 Si1 F1 93.01(6) . . ? F4 Si1 F1 92.68(5) . . ? F2 Si1 F1 171.10(6) . . ? F3 Si1 N1 89.72(6) . . ? F4 Si1 N1 173.53(7) . . ? F2 Si1 N1 88.29(6) . . ? F1 Si1 N1 84.94(7) . . ? F3 Si1 N2 174.80(6) . . ? F4 Si1 N2 88.77(6) . . ? F2 Si1 N2 86.62(6) . . ? F1 Si1 N2 87.05(6) . . ? N1 Si1 N2 85.10(7) . . ? C3 N1 C1 109.35(15) . . ? C3 N1 C2 108.16(15) . . ? C1 N1 C2 106.28(14) . . ? C3 N1 Si1 106.65(11) . . ? C1 N1 Si1 113.93(12) . . ? C2 N1 Si1 112.35(12) . . ? C5 N2 C4 107.83(14) . . ? C5 N2 C6 106.52(14) . . ? C4 N2 C6 109.54(15) . . ? C5 N2 Si1 112.80(12) . . ? C4 N2 Si1 108.22(10) . . ? C6 N2 Si1 111.83(11) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 108.32(16) . . ? N1 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N1 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N2 C4 C3 108.77(15) . . ? N2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # F4 Si1 N1 C3 -0.3(7) . . . . ? # F4 Si1 N1 C1 120.5(6) . . . . ? # F4 Si1 N1 C2 -118.6(6) . . . . ? # F3 Si1 N2 C5 -122.5(7) . . . . ? # F3 Si1 N2 C4 -3.3(8) . . . . ? # F3 Si1 N2 C6 117.5(7) . . . . ? F3 Si1 N1 C3 161.41(12) . . . . ? F2 Si1 N1 C3 -105.85(12) . . . . ? F1 Si1 N1 C3 68.37(12) . . . . ? N2 Si1 N1 C3 -19.10(12) . . . . ? F3 Si1 N1 C1 -77.85(13) . . . . ? F2 Si1 N1 C1 14.89(13) . . . . ? F1 Si1 N1 C1 -170.89(13) . . . . ? N2 Si1 N1 C1 101.64(13) . . . . ? F3 Si1 N1 C2 43.08(12) . . . . ? F2 Si1 N1 C2 135.82(12) . . . . ? F1 Si1 N1 C2 -49.97(12) . . . . ? N2 Si1 N1 C2 -137.43(12) . . . . ? F4 Si1 N2 C5 53.98(13) . . . . ? F2 Si1 N2 C5 -39.53(12) . . . . ? F1 Si1 N2 C5 146.72(12) . . . . ? N1 Si1 N2 C5 -128.11(12) . . . . ? F4 Si1 N2 C4 173.19(13) . . . . ? F2 Si1 N2 C4 79.68(12) . . . . ? F1 Si1 N2 C4 -94.06(13) . . . . ? N1 Si1 N2 C4 -8.89(13) . . . . ? F4 Si1 N2 C6 -66.07(13) . . . . ? F2 Si1 N2 C6 -159.58(13) . . . . ? F1 Si1 N2 C6 26.67(13) . . . . ? N1 Si1 N2 C6 111.84(14) . . . . ? C1 N1 C3 C4 -80.05(18) . . . . ? C2 N1 C3 C4 164.62(15) . . . . ? Si1 N1 C3 C4 43.57(16) . . . . ? C5 N2 C4 C3 157.56(15) . . . . ? C6 N2 C4 C3 -86.90(18) . . . . ? Si1 N2 C4 C3 35.25(17) . . . . ? N1 C3 C4 N2 -53.06(18) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.284 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.044 #===END OF CIF ============================================================== # 08wz1104 data_08wz1104 _database_code_depnum_ccdc_archive 'CCDC 713186' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-11-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrafluorosilicon(IV)-N-(chloromethyl)-2- {[2-(dimethylamino)ethyl](methyl)amino}-N,N-dimethylethanaminium pentafluorosilicon(IV) ; # iLab N3 ligand name: # N-(chloromethyl)-2-{[2-(dimethylamino)ethyl](methyl)amino}- # N,N-dimethylethanaminium _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H25 Cl F4 N3 Si 1+, F5 Si 1-' _chemical_formula_sum 'C10 H25 Cl F9 N3 Si2' _chemical_formula_structural '((C10 H25 Cl N3) (F4 Si)) (F5 Si)' _chemical_formula_weight 449.96 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' 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' Cl Cl 0.1484 0.1585 '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' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9707(15) _cell_length_b 11.533(2) _cell_length_c 12.264(2) _cell_angle_alpha 107.672(10) _cell_angle_beta 95.625(10) _cell_angle_gamma 98.336(10) _cell_volume 918.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 22305 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7178 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17682 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.57 _reflns_number_total 4177 _reflns_number_gt 2895 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+3.7402P] 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 4177 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2366 _refine_ls_wR_factor_gt 0.2012 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Cl1 Cl 0.4675(2) 0.59109(14) 0.15526(13) 0.0446(4) Uani 1 1 d . . . Si1 Si 0.64058(19) 0.23045(11) 0.43106(11) 0.0245(3) Uani 1 1 d . . . Si2 Si 0.0426(2) 0.77899(14) 0.03130(12) 0.0332(4) Uani 1 1 d . . . F1 F 0.7459(5) 0.1882(3) 0.5342(2) 0.0354(7) Uani 1 1 d . . . F2 F 0.6182(4) 0.3688(2) 0.5155(2) 0.0301(6) Uani 1 1 d . . . F3 F 0.4189(4) 0.1668(3) 0.4413(2) 0.0323(7) Uani 1 1 d . . . F4 F 0.8506(4) 0.2894(2) 0.3993(2) 0.0278(6) Uani 1 1 d . . . F5 F 0.1041(8) 0.6457(4) 0.0115(4) 0.0711(13) Uani 1 1 d . . . F6 F 0.2045(9) 0.8970(4) 0.0551(4) 0.096(2) Uani 1 1 d . . . F7 F -0.1863(6) 0.7814(5) 0.0268(4) 0.0710(13) Uani 1 1 d . . . F8 F 0.0587(6) 0.7978(4) 0.1712(3) 0.0533(10) Uani 1 1 d . . . F9 F 0.0250(6) 0.7567(4) -0.1090(3) 0.0510(9) Uani 1 1 d . . . N1 N 0.6640(6) 0.0675(4) 0.3146(4) 0.0287(9) Uani 1 1 d . . . N2 N 0.5018(6) 0.2683(4) 0.2922(3) 0.0292(9) Uani 1 1 d . . . N3 N 0.7986(6) 0.5744(4) 0.2825(3) 0.0255(8) Uani 1 1 d . . . C1 C 0.8649(9) 0.0395(6) 0.3264(6) 0.0469(15) Uani 1 1 d . . . H1A H 0.8943 0.0249 0.4004 0.070 Uiso 1 1 calc R . . H1B H 0.9600 0.1098 0.3238 0.070 Uiso 1 1 calc R . . H1C H 0.8731 -0.0345 0.2627 0.070 Uiso 1 1 calc R . . C2 C 0.5281(9) -0.0413(4) 0.3253(5) 0.0367(12) Uani 1 1 d . . . H2A H 0.5504 -0.1179 0.2701 0.055 Uiso 1 1 calc R . . H2B H 0.3918 -0.0321 0.3086 0.055 Uiso 1 1 calc R . . H2C H 0.5537 -0.0447 0.4042 0.055 Uiso 1 1 calc R . . C3 C 0.6140(9) 0.0775(5) 0.1959(4) 0.0381(13) Uani 1 1 d . . . H3A H 0.7284 0.1236 0.1753 0.046 Uiso 1 1 calc R . . H3B H 0.5777 -0.0060 0.1375 0.046 Uiso 1 1 calc R . . C4 C 0.4455(10) 0.1446(5) 0.1984(5) 0.0419(14) Uani 1 1 d . . . H4A H 0.3288 0.0955 0.2139 0.050 Uiso 1 1 calc R . . H4B H 0.4128 0.1564 0.1226 0.050 Uiso 1 1 calc R . . C5 C 0.3175(8) 0.3170(5) 0.3191(6) 0.0436(14) Uani 1 1 d . . . H5A H 0.3483 0.3905 0.3884 0.065 Uiso 1 1 calc R . . H5B H 0.2232 0.2532 0.3329 0.065 Uiso 1 1 calc R . . H5C H 0.2606 0.3392 0.2536 0.065 Uiso 1 1 calc R . . C6 C 0.6224(8) 0.3541(4) 0.2442(4) 0.0316(11) Uani 1 1 d . . . H6A H 0.5474 0.3561 0.1721 0.038 Uiso 1 1 calc R . . H6B H 0.7433 0.3222 0.2244 0.038 Uiso 1 1 calc R . . C7 C 0.6779(8) 0.4853(4) 0.3301(4) 0.0301(11) Uani 1 1 d . . . H7A H 0.5567 0.5164 0.3506 0.036 Uiso 1 1 calc R . . H7B H 0.7538 0.4830 0.4018 0.036 Uiso 1 1 calc R . . C8 C 1.0036(8) 0.5471(5) 0.2729(5) 0.0365(12) Uani 1 1 d . . . H8A H 0.9966 0.4667 0.2137 0.055 Uiso 1 1 calc R . . H8B H 1.0647 0.5451 0.3476 0.055 Uiso 1 1 calc R . . H8C H 1.0823 0.6119 0.2512 0.055 Uiso 1 1 calc R . . C9 C 0.8153(8) 0.7021(4) 0.3663(4) 0.0303(10) Uani 1 1 d . . . H9A H 0.9031 0.7611 0.3424 0.045 Uiso 1 1 calc R . . H9B H 0.8683 0.7037 0.4439 0.045 Uiso 1 1 calc R . . H9C H 0.6853 0.7250 0.3675 0.045 Uiso 1 1 calc R . . C10 C 0.7125(8) 0.5689(5) 0.1633(4) 0.0350(11) Uani 1 1 d . . . H10A H 0.7186 0.4873 0.1077 0.042 Uiso 1 1 calc R . . H10B H 0.7926 0.6333 0.1404 0.042 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 Cl1 0.0383(7) 0.0483(8) 0.0465(8) 0.0143(6) -0.0004(6) 0.0131(6) Si1 0.0266(7) 0.0199(6) 0.0247(6) 0.0046(5) 0.0050(5) 0.0016(5) Si2 0.0363(8) 0.0319(7) 0.0278(7) 0.0049(6) 0.0084(6) 0.0025(6) F1 0.0458(18) 0.0316(15) 0.0277(15) 0.0108(12) 0.0027(13) 0.0027(13) F2 0.0340(15) 0.0229(13) 0.0265(14) -0.0007(11) 0.0037(12) 0.0027(11) F3 0.0320(15) 0.0256(14) 0.0345(15) 0.0029(12) 0.0138(12) -0.0008(12) F4 0.0254(14) 0.0231(13) 0.0326(14) 0.0069(11) 0.0062(11) 0.0010(11) F5 0.102(4) 0.057(2) 0.056(2) 0.0096(19) 0.011(2) 0.039(2) F6 0.132(5) 0.072(3) 0.051(2) 0.018(2) -0.015(3) -0.066(3) F7 0.045(2) 0.115(4) 0.078(3) 0.055(3) 0.026(2) 0.031(2) F8 0.072(3) 0.055(2) 0.0323(17) 0.0124(16) 0.0127(17) 0.0107(19) F9 0.053(2) 0.059(2) 0.0319(17) 0.0057(15) 0.0030(15) 0.0019(17) N1 0.034(2) 0.0223(19) 0.030(2) 0.0078(16) 0.0111(17) 0.0040(17) N2 0.034(2) 0.0192(19) 0.027(2) 0.0002(16) -0.0042(17) 0.0009(16) N3 0.029(2) 0.0213(19) 0.0253(19) 0.0049(15) 0.0059(16) 0.0067(16) C1 0.039(3) 0.038(3) 0.061(4) 0.009(3) 0.010(3) 0.012(3) C2 0.049(3) 0.019(2) 0.038(3) 0.006(2) 0.013(2) -0.003(2) C3 0.057(4) 0.025(2) 0.026(2) 0.0025(19) 0.012(2) -0.003(2) C4 0.061(4) 0.024(3) 0.026(3) -0.004(2) -0.010(2) 0.001(2) C5 0.033(3) 0.033(3) 0.057(4) 0.009(3) -0.006(3) 0.004(2) C6 0.048(3) 0.022(2) 0.023(2) 0.0053(18) 0.002(2) 0.007(2) C7 0.042(3) 0.023(2) 0.025(2) 0.0062(19) 0.010(2) 0.007(2) C8 0.027(3) 0.034(3) 0.044(3) 0.003(2) 0.003(2) 0.009(2) C9 0.036(3) 0.021(2) 0.031(2) 0.0045(19) 0.007(2) 0.0038(19) C10 0.033(3) 0.042(3) 0.030(3) 0.012(2) 0.002(2) 0.009(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 Cl1 C10 1.761(5) . ? Si1 F1 1.634(3) . ? Si1 F3 1.645(3) . ? Si1 F4 1.655(3) . ? Si1 F2 1.656(3) . ? Si1 N1 2.026(4) . ? Si1 N2 2.069(4) . ? Si2 F6 1.568(4) . ? Si2 F7 1.596(4) . ? Si2 F5 1.609(4) . ? Si2 F9 1.650(4) . ? Si2 F8 1.653(4) . ? N1 C1 1.485(7) . ? N1 C3 1.506(7) . ? N1 C2 1.506(6) . ? N2 C6 1.497(7) . ? N2 C5 1.502(7) . ? N2 C4 1.505(6) . ? N3 C9 1.500(6) . ? N3 C10 1.504(6) . ? N3 C8 1.515(6) . ? N3 C7 1.521(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.495(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.527(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? 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 Si1 F3 93.54(17) . . ? F1 Si1 F4 94.02(16) . . ? F3 Si1 F4 171.15(16) . . ? F1 Si1 F2 95.87(16) . . ? F3 Si1 F2 92.76(15) . . ? F4 Si1 F2 91.05(15) . . ? F1 Si1 N1 89.42(17) . . ? F3 Si1 N1 88.63(16) . . ? F4 Si1 N1 86.84(16) . . ? F2 Si1 N1 174.43(17) . . ? F1 Si1 N2 175.16(17) . . ? F3 Si1 N2 84.73(17) . . ? F4 Si1 N2 87.37(17) . . ? F2 Si1 N2 88.73(16) . . ? N1 Si1 N2 86.02(17) . . ? F6 Si2 F7 123.9(3) . . ? F6 Si2 F5 119.9(3) . . ? F7 Si2 F5 116.1(3) . . ? F6 Si2 F9 89.9(2) . . ? F7 Si2 F9 90.8(2) . . ? F5 Si2 F9 90.1(2) . . ? F6 Si2 F8 91.2(2) . . ? F7 Si2 F8 89.2(2) . . ? F5 Si2 F8 88.8(2) . . ? F9 Si2 F8 178.7(2) . . ? C1 N1 C3 108.7(4) . . ? C1 N1 C2 106.3(4) . . ? C3 N1 C2 109.2(4) . . ? C1 N1 Si1 112.5(3) . . ? C3 N1 Si1 107.2(3) . . ? C2 N1 Si1 112.8(3) . . ? C6 N2 C5 108.2(4) . . ? C6 N2 C4 107.4(4) . . ? C5 N2 C4 108.2(4) . . ? C6 N2 Si1 116.5(3) . . ? C5 N2 Si1 111.7(3) . . ? C4 N2 Si1 104.5(3) . . ? C9 N3 C10 110.4(4) . . ? C9 N3 C8 108.2(4) . . ? C10 N3 C8 105.9(4) . . ? C9 N3 C7 107.2(3) . . ? C10 N3 C7 113.5(4) . . ? C8 N3 C7 111.6(4) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 107.8(4) . . ? C4 C3 H3A 110.2 . . ? N1 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? N1 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 N2 108.8(4) . . ? C3 C4 H4A 109.9 . . ? N2 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? N2 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.9(4) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C6 112.7(4) . . ? N3 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N3 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 Cl1 112.7(4) . . ? N3 C10 H10A 109.1 . . ? Cl1 C10 H10A 109.1 . . ? N3 C10 H10B 109.1 . . ? Cl1 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 N2 56.9(6) . . . . ? N2 C6 C7 N3 -179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.630 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.136 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================