#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/91/2239121.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2239121 loop_ _publ_author_name 'Ouasri, Ali' 'Rhandour, Ali' 'Saadi, Mohamed' 'El Ammari, Lahcen' _publ_section_title ; Hexane-1,6-diammonium hexafluorosilicate ; _journal_coeditor_code RZ5101 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o92 _journal_page_last o93 _journal_paper_doi 10.1107/S1600536813034144 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C6 H18 N2 2+, Si F6 2-' _chemical_formula_moiety 'C6 H18 N2 2+, F6 Si 2-' _chemical_formula_sum 'C6 H18 F6 N2 Si' _chemical_formula_weight 260.31 _chemical_name_systematic ; Hexane-1,6-diammonium hexafluorosilicate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 91.379(2) _cell_angle_beta 92.797(2) _cell_angle_gamma 90.906(2) _cell_formula_units_Z 4 _cell_length_a 5.8965(2) _cell_length_b 13.6946(5) _cell_length_c 14.4945(5) _cell_measurement_reflns_used 4760 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 2.02 _cell_volume 1168.53(7) _computing_cell_refinement 'SAINT-Plus (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT-Plus (Bruker, 2009)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'PLATON (Spek, 2009) and publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 29127 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.02 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_correction_T_min 0.6855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.458 _refine_diff_density_min -0.264 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 4760 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0515 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+1.0436P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1456 _refine_ls_wR_factor_ref 0.1593 _reflns_number_gt 3618 _reflns_number_total 4760 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL EL_RHC6Si in P-1 CELL 0.71073 5.8965 13.6946 14.4945 91.379 92.797 90.906 ZERR 2.00 0.0002 0.0005 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N F SI UNIT 24 72 8 24 4 MERG 2 OMIT 0 1 0 OMIT 0 0 1 OMIT 0 1 1 OMIT 1 -1 1 SHEL 40 0.8 FMAP 2 PLAN 10 ACTA BOND BOND $H HTAB 2.6 HTAB N2 F1 HTAB N2 F5 HTAB N2 F6 HTAB N2 F7 HTAB N2 F8 HTAB N3 F1 HTAB N3 F2 HTAB N4 F7 HTAB N4 F8 HTAB N4 F9 HTAB N4 F1 HTAB N4 F2 HTAB N4 F6 EQIV $1 -x, -y+2, -z+1 EQIV $2 x, y, z+1 EQIV $3 -x+1, -y+2, -z+1 EQIV $4 -x, -y+1, -z+1 EQIV $5 x+1, y, z EQIV $6 x-1, y, z EQIV $7 x+1, y, z+1 EQIV $8 -x+1, -y+1, -z+1 EQIV $9 -x, -y+2, -z HTAB N1 F11_$1 HTAB N1 F12_$2 HTAB N1 F10_$3 HTAB N1 F11_$7 HTAB N1 F2_$2 HTAB N1 F3_$2 HTAB N2 F7_$8 HTAB N2 F8_$5 HTAB N2 F9_$5 HTAB N2 F9_$4 HTAB N3 F10_$9 HTAB N3 F12 HTAB N3 F3_$6 HTAB N3 F4_$6 HTAB N3 F5_$6 HTAB N4 F4_$6 HTAB N4 F5_$6 L.S. 10 TEMP 23.00 size 0.37 0.33 0.28 WGHT 0.073400 1.043600 FVAR 0.14249 C1 1 0.459982 0.754131 0.970243 11.00000 0.08435 0.05423 = 0.04151 -0.00454 0.00831 -0.00965 AFIX 23 H1A 2 0.299715 0.736664 0.968150 11.00000 -1.20000 H1B 2 0.542516 0.701841 0.999988 11.00000 -1.20000 AFIX 0 C2 1 0.535300 0.763193 0.873401 11.00000 0.08091 0.06402 = 0.04485 -0.00580 0.01262 -0.00934 AFIX 23 H2A 2 0.456081 0.816786 0.844333 11.00000 -1.20000 H2B 2 0.696525 0.778818 0.875514 11.00000 -1.20000 AFIX 0 C3 1 0.491708 0.671979 0.815765 11.00000 0.12812 0.05750 = 0.04625 -0.00312 0.00746 -0.00244 AFIX 23 H3A 2 0.329501 0.658464 0.811726 11.00000 -1.20000 H3B 2 0.563835 0.618021 0.847137 11.00000 -1.20000 AFIX 0 C4 1 0.576026 0.675427 0.717935 11.00000 0.11784 0.08138 = 0.04993 -0.00121 0.00465 0.02542 AFIX 23 H4A 2 0.736559 0.692469 0.722148 11.00000 -1.20000 H4B 2 0.560846 0.610344 0.690185 11.00000 -1.20000 AFIX 0 C5 1 0.460421 0.743721 0.655794 11.00000 0.10504 0.06730 = 0.04879 -0.01036 -0.00067 0.01572 AFIX 23 H5A 2 0.471788 0.808320 0.684761 11.00000 -1.20000 H5B 2 0.300614 0.725445 0.650675 11.00000 -1.20000 AFIX 0 C6 1 0.543268 0.750797 0.559981 11.00000 0.09156 0.05057 = 0.04478 -0.00226 0.00470 -0.00893 AFIX 23 H6A 2 0.466119 0.803907 0.529229 11.00000 -1.20000 H6B 2 0.704311 0.766854 0.564186 11.00000 -1.20000 AFIX 0 C7 1 0.051632 1.037038 0.285714 11.00000 0.07277 0.04113 = 0.04279 0.00201 0.00371 -0.00566 AFIX 23 H7A 2 -0.015064 1.083406 0.243188 11.00000 -1.20000 H7B 2 0.213330 1.051282 0.292545 11.00000 -1.20000 AFIX 0 C8 1 -0.050585 1.049829 0.377525 11.00000 0.07620 0.04583 = 0.04310 -0.00745 0.00047 0.00888 AFIX 23 H8A 2 -0.210993 1.033023 0.370264 11.00000 -1.20000 H8B 2 -0.038297 1.118353 0.395923 11.00000 -1.20000 AFIX 0 C9 1 0.053048 0.990568 0.454504 11.00000 0.07356 0.05507 = 0.03669 -0.00841 0.00215 0.00946 AFIX 23 H9A 2 0.035831 0.921716 0.437908 11.00000 -1.20000 H9B 2 0.214295 1.005778 0.461440 11.00000 -1.20000 AFIX 0 C10 1 -0.054542 0.546520 0.212537 11.00000 0.06672 0.04241 = 0.04000 -0.00434 0.00856 -0.00722 AFIX 23 H10A 2 -0.218257 0.537673 0.207491 11.00000 -1.20000 H10B 2 0.010399 0.485970 0.233897 11.00000 -1.20000 AFIX 0 C11 1 0.029174 0.567527 0.119710 11.00000 0.06803 0.05133 = 0.03776 -0.00739 0.00983 -0.00851 AFIX 23 H11A 2 0.193647 0.572434 0.124273 11.00000 -1.20000 H11B 2 -0.027902 0.630227 0.100338 11.00000 -1.20000 AFIX 0 C12 1 -0.041658 0.490824 0.047108 11.00000 0.08464 0.05959 = 0.04069 -0.01146 0.01369 -0.01710 AFIX 23 H12A 2 0.013855 0.428137 0.067240 11.00000 -1.20000 H12B 2 -0.206192 0.486424 0.042620 11.00000 -1.20000 AFIX 0 N1 3 0.496981 0.844531 1.025540 11.00000 0.03427 0.04771 = 0.02835 0.00551 0.00309 -0.00054 AFIX 33 H1NB 2 0.444201 0.894782 0.993653 11.00000 -1.20000 H1NA 2 0.644912 0.853501 1.038823 11.00000 -1.20000 H1NC 2 0.424292 0.840190 1.077713 11.00000 -1.20000 AFIX 0 N2 3 0.507294 0.661283 0.503326 11.00000 0.03272 0.04389 = 0.03118 0.00504 0.00459 0.00268 AFIX 33 H2NA 2 0.582354 0.612606 0.529758 11.00000 -1.20000 H2NC 2 0.557966 0.670622 0.447319 11.00000 -1.20000 H2NB 2 0.359718 0.646266 0.498499 11.00000 -1.20000 AFIX 0 N3 3 0.015867 0.937118 0.246368 11.00000 0.03493 0.04093 = 0.02671 0.00227 0.00303 0.00202 AFIX 33 H3NA 2 0.087737 0.894779 0.282588 11.00000 -1.20000 H3NB 2 0.070318 0.933815 0.190202 11.00000 -1.20000 H3NC 2 -0.131995 0.922581 0.242618 11.00000 -1.20000 AFIX 0 N4 3 0.003899 0.624789 0.280627 11.00000 0.03195 0.03747 = 0.02888 0.00323 0.00380 0.00205 AFIX 33 H4NA 2 -0.053865 0.610402 0.334340 11.00000 -1.20000 H4NB 2 -0.053172 0.680757 0.260863 11.00000 -1.20000 H4NC 2 0.154241 0.630759 0.288047 11.00000 -1.20000 AFIX 0 F1 4 0.305672 0.800634 0.348864 11.00000 0.03762 0.06808 = 0.03729 0.00802 0.01242 0.01173 F2 4 0.306006 0.771366 0.188096 11.00000 0.03246 0.06263 = 0.03590 0.00822 -0.00237 0.00110 F3 4 0.530572 0.901857 0.254877 11.00000 0.04349 0.04346 = 0.07987 0.01612 0.00454 0.00109 F4 4 0.709609 0.761755 0.196504 11.00000 0.03396 0.06811 = 0.04311 0.01885 0.01485 0.01194 F5 4 0.712194 0.790063 0.357855 11.00000 0.03628 0.08567 = 0.04543 0.00993 -0.00837 0.00079 F6 4 0.488164 0.660264 0.291724 11.00000 0.04249 0.04211 = 0.06622 0.02123 0.01179 0.00620 F7 4 0.202972 0.490658 0.422531 11.00000 0.03713 0.06347 = 0.04678 0.01710 0.01783 0.01068 F8 4 0.018784 0.622644 0.494281 11.00000 0.04652 0.03886 = 0.07080 0.01493 0.01038 0.00312 F9 4 -0.202467 0.499352 0.414887 11.00000 0.03584 0.07435 = 0.04429 0.01779 -0.00399 -0.00014 F10 4 0.022594 1.118433 -0.027638 11.00000 0.04277 0.05823 = 0.07261 0.02682 0.00341 -0.00075 F11 4 -0.196324 1.027340 0.076613 11.00000 0.03512 0.08583 = 0.03657 0.01577 0.00900 0.01195 F12 4 0.208669 1.015086 0.082064 11.00000 0.03112 0.08230 = 0.03797 0.01211 -0.00524 -0.00170 SI1 5 0.509216 0.781572 0.273665 11.00000 0.02457 0.04306 = 0.03176 0.01261 0.00396 0.00350 SI2 5 0.000000 0.500000 0.500000 10.50000 0.02499 0.04105 = 0.03681 0.01419 0.00672 0.00386 SI3 5 0.000000 1.000000 0.000000 10.50000 0.02442 0.05750 = 0.02981 0.01662 0.00217 0.00112 HKLF 4 REM EL_RHC6Si in P-1 REM R1 = 0.0515 for 3614 Fo > 4sig(Fo) and 0.0682 for all 4760 data REM 274 parameters refined using 0 restraints END WGHT 0.0734 1.0472 REM Highest difference peak 0.458, deepest hole -0.264, 1-sigma level 0.069 Q1 1 0.6216 0.7251 0.6580 11.00000 0.05 0.46 Q2 1 0.3885 0.6885 0.7047 11.00000 0.05 0.46 Q3 1 0.0901 0.5427 0.2106 11.00000 0.05 0.44 Q4 1 0.4553 0.7451 0.8133 11.00000 0.05 0.39 Q5 1 0.5357 0.7428 0.7344 11.00000 0.05 0.37 Q6 1 0.5462 0.7003 0.9067 11.00000 0.05 0.35 Q7 1 0.4836 0.7579 0.2014 11.00000 0.05 0.35 Q8 1 0.6714 0.7868 0.3017 11.00000 0.05 0.34 Q9 1 0.4680 0.8019 0.3419 11.00000 0.05 0.33 Q10 1 0.4709 0.8786 0.2252 11.00000 0.05 0.32 ; _cod_data_source_file rz5101sup1.cf _cod_data_source_block I _cod_database_code 2239121 _cod_database_fobs_code 2239121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity C C1 0.4600(7) 0.7541(2) 0.9702(2) 0.0601(9) Uani d . 1 1 H H1A 0.2997 0.7367 0.9682 0.072 Uiso calc R 1 1 H H1B 0.5425 0.7018 1.0000 0.072 Uiso calc R 1 1 C C2 0.5353(7) 0.7632(3) 0.8734(2) 0.0632(9) Uani d . 1 1 H H2A 0.4561 0.8168 0.8443 0.076 Uiso calc R 1 1 H H2B 0.6965 0.7788 0.8755 0.076 Uiso calc R 1 1 C C3 0.4917(8) 0.6720(3) 0.8158(2) 0.0773(12) Uani d . 1 1 H H3A 0.3295 0.6585 0.8117 0.093 Uiso calc R 1 1 H H3B 0.5638 0.6180 0.8471 0.093 Uiso calc R 1 1 C C4 0.5760(8) 0.6754(3) 0.7179(2) 0.0828(12) Uani d . 1 1 H H4A 0.7366 0.6925 0.7221 0.099 Uiso calc R 1 1 H H4B 0.5608 0.6103 0.6902 0.099 Uiso calc R 1 1 C C5 0.4604(8) 0.7437(3) 0.6558(2) 0.0739(11) Uani d . 1 1 H H5A 0.4718 0.8083 0.6848 0.089 Uiso calc R 1 1 H H5B 0.3006 0.7254 0.6507 0.089 Uiso calc R 1 1 C C6 0.5433(7) 0.7508(2) 0.5600(2) 0.0624(9) Uani d . 1 1 H H6A 0.4661 0.8039 0.5292 0.075 Uiso calc R 1 1 H H6B 0.7043 0.7669 0.5642 0.075 Uiso calc R 1 1 C C7 0.0516(6) 1.0370(2) 0.2857(2) 0.0523(7) Uani d . 1 1 H H7A -0.0151 1.0834 0.2432 0.063 Uiso calc R 1 1 H H7B 0.2133 1.0513 0.2925 0.063 Uiso calc R 1 1 C C8 -0.0506(6) 1.0498(2) 0.3775(2) 0.0552(8) Uani d . 1 1 H H8A -0.2110 1.0330 0.3703 0.066 Uiso calc R 1 1 H H8B -0.0383 1.1184 0.3959 0.066 Uiso calc R 1 1 C C9 0.0530(6) 0.9906(2) 0.45450(19) 0.0552(8) Uani d . 1 1 H H9A 0.0358 0.9217 0.4379 0.066 Uiso calc R 1 1 H H9B 0.2143 1.0058 0.4614 0.066 Uiso calc R 1 1 C C10 -0.0545(6) 0.5465(2) 0.21254(19) 0.0497(7) Uani d . 1 1 H H10A -0.2183 0.5377 0.2075 0.060 Uiso calc R 1 1 H H10B 0.0104 0.4860 0.2339 0.060 Uiso calc R 1 1 C C11 0.0292(6) 0.5675(2) 0.11971(19) 0.0524(7) Uani d . 1 1 H H11A 0.1936 0.5724 0.1243 0.063 Uiso calc R 1 1 H H11B -0.0279 0.6302 0.1003 0.063 Uiso calc R 1 1 C C12 -0.0417(7) 0.4908(3) 0.0471(2) 0.0617(9) Uani d . 1 1 H H12A 0.0139 0.4281 0.0672 0.074 Uiso calc R 1 1 H H12B -0.2062 0.4864 0.0426 0.074 Uiso calc R 1 1 N N1 0.4970(3) 0.84453(16) 1.02554(13) 0.0367(5) Uani d . 1 1 H H1NB 0.4442 0.8948 0.9937 0.044 Uiso calc R 1 1 H H1NA 0.6449 0.8535 1.0388 0.044 Uiso calc R 1 1 H H1NC 0.4243 0.8402 1.0777 0.044 Uiso calc R 1 1 N N2 0.5073(3) 0.66128(16) 0.50333(14) 0.0357(5) Uani d . 1 1 H H2NA 0.5824 0.6126 0.5298 0.043 Uiso calc R 1 1 H H2NC 0.5580 0.6706 0.4473 0.043 Uiso calc R 1 1 H H2NB 0.3597 0.6463 0.4985 0.043 Uiso calc R 1 1 N N3 0.0159(3) 0.93712(15) 0.24637(13) 0.0341(5) Uani d . 1 1 H H3NA 0.0877 0.8948 0.2826 0.041 Uiso calc R 1 1 H H3NB 0.0703 0.9338 0.1902 0.041 Uiso calc R 1 1 H H3NC -0.1320 0.9226 0.2426 0.041 Uiso calc R 1 1 N N4 0.0039(3) 0.62479(15) 0.28063(13) 0.0326(4) Uani d . 1 1 H H4NA -0.0539 0.6104 0.3343 0.039 Uiso calc R 1 1 H H4NB -0.0532 0.6808 0.2609 0.039 Uiso calc R 1 1 H H4NC 0.1542 0.6308 0.2880 0.039 Uiso calc R 1 1 F F1 0.3057(2) 0.80063(13) 0.34886(10) 0.0471(4) Uani d . 1 1 F F2 0.3060(2) 0.77137(12) 0.18810(10) 0.0437(4) Uani d . 1 1 F F3 0.5306(3) 0.90186(12) 0.25488(13) 0.0553(5) Uani d . 1 1 F F4 0.7096(2) 0.76175(13) 0.19650(11) 0.0476(4) Uani d . 1 1 F F5 0.7122(3) 0.79006(15) 0.35786(11) 0.0560(5) Uani d . 1 1 F F6 0.4882(3) 0.66026(12) 0.29172(12) 0.0496(4) Uani d . 1 1 F F7 0.2030(2) 0.49066(13) 0.42253(11) 0.0483(4) Uani d . 1 1 F F8 0.0188(3) 0.62264(11) 0.49428(12) 0.0516(4) Uani d . 1 1 F F9 -0.2025(3) 0.49935(13) 0.41489(11) 0.0514(4) Uani d . 1 1 F F10 0.0226(3) 1.11843(13) -0.02764(13) 0.0575(5) Uani d . 1 1 F F11 -0.1963(2) 1.02734(14) 0.07661(10) 0.0519(5) Uani d . 1 1 F F12 0.2087(2) 1.01509(14) 0.08206(10) 0.0505(4) Uani d . 1 1 Si Si1 0.50922(10) 0.78157(5) 0.27367(5) 0.0328(2) Uani d . 1 1 Si Si2 0.0000 0.5000 0.5000 0.0339(2) Uani d S 1 2 Si Si3 0.0000 1.0000 0.0000 0.0370(3) Uani d S 1 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.084(2) 0.0542(19) 0.0415(16) -0.0097(17) 0.0083(15) -0.0045(14) C2 0.081(2) 0.064(2) 0.0448(17) -0.0093(18) 0.0126(16) -0.0058(15) C3 0.128(4) 0.057(2) 0.0463(19) -0.002(2) 0.007(2) -0.0031(16) C4 0.118(3) 0.081(3) 0.050(2) 0.025(2) 0.005(2) -0.0012(19) C5 0.105(3) 0.067(2) 0.0488(19) 0.016(2) -0.0007(19) -0.0104(17) C6 0.092(3) 0.0506(19) 0.0448(17) -0.0089(17) 0.0047(16) -0.0023(14) C7 0.073(2) 0.0411(16) 0.0428(16) -0.0057(14) 0.0037(14) 0.0020(12) C8 0.076(2) 0.0458(17) 0.0431(16) 0.0089(15) 0.0005(14) -0.0075(13) C9 0.074(2) 0.0551(19) 0.0367(15) 0.0095(16) 0.0021(14) -0.0084(13) C10 0.0667(19) 0.0424(16) 0.0400(15) -0.0072(14) 0.0086(13) -0.0043(12) C11 0.068(2) 0.0513(18) 0.0378(15) -0.0085(15) 0.0098(13) -0.0074(13) C12 0.085(2) 0.060(2) 0.0407(17) -0.0171(18) 0.0137(16) -0.0115(14) N1 0.0343(11) 0.0477(13) 0.0284(10) -0.0005(9) 0.0031(8) 0.0055(9) N2 0.0327(11) 0.0439(12) 0.0312(10) 0.0027(9) 0.0046(8) 0.0050(9) N3 0.0349(11) 0.0409(12) 0.0267(10) 0.0020(9) 0.0030(8) 0.0023(8) N4 0.0320(10) 0.0375(11) 0.0289(10) 0.0021(8) 0.0038(8) 0.0032(8) F1 0.0376(8) 0.0681(11) 0.0373(8) 0.0117(7) 0.0124(6) 0.0080(7) F2 0.0325(8) 0.0626(10) 0.0359(8) 0.0011(7) -0.0024(6) 0.0082(7) F3 0.0435(9) 0.0435(9) 0.0799(12) 0.0011(7) 0.0045(8) 0.0161(8) F4 0.0340(8) 0.0681(11) 0.0431(9) 0.0119(7) 0.0149(6) 0.0189(8) F5 0.0363(8) 0.0857(13) 0.0454(9) 0.0008(8) -0.0084(7) 0.0099(9) F6 0.0425(9) 0.0421(9) 0.0662(11) 0.0062(7) 0.0118(7) 0.0212(8) F7 0.0371(8) 0.0635(11) 0.0468(9) 0.0107(7) 0.0178(7) 0.0171(8) F8 0.0465(9) 0.0389(9) 0.0708(11) 0.0031(7) 0.0104(8) 0.0149(8) F9 0.0358(8) 0.0743(12) 0.0443(9) -0.0001(8) -0.0040(7) 0.0178(8) F10 0.0428(9) 0.0582(11) 0.0726(12) -0.0008(8) 0.0034(8) 0.0268(9) F11 0.0351(8) 0.0858(13) 0.0366(8) 0.0119(8) 0.0090(6) 0.0158(8) F12 0.0311(8) 0.0823(13) 0.0380(8) -0.0017(8) -0.0052(6) 0.0121(8) Si1 0.0246(3) 0.0431(4) 0.0318(4) 0.0035(3) 0.0040(3) 0.0126(3) Si2 0.0250(5) 0.0411(6) 0.0368(5) 0.0039(4) 0.0067(4) 0.0142(4) Si3 0.0244(5) 0.0575(7) 0.0298(5) 0.0011(4) 0.0022(4) 0.0166(4) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle N1 C1 C2 . . 112.6(3) N1 C1 H1A . . 109.1 C2 C1 H1A . . 109.1 N1 C1 H1B . . 109.1 C2 C1 H1B . . 109.1 H1A C1 H1B . . 107.8 C3 C2 C1 . . 112.9(3) C3 C2 H2A . . 109.0 C1 C2 H2A . . 109.0 C3 C2 H2B . . 109.0 C1 C2 H2B . . 109.0 H2A C2 H2B . . 107.8 C2 C3 C4 . . 115.1(3) C2 C3 H3A . . 108.5 C4 C3 H3A . . 108.5 C2 C3 H3B . . 108.5 C4 C3 H3B . . 108.5 H3A C3 H3B . . 107.5 C5 C4 C3 . . 116.0(3) C5 C4 H4A . . 108.3 C3 C4 H4A . . 108.3 C5 C4 H4B . . 108.3 C3 C4 H4B . . 108.3 H4A C4 H4B . . 107.4 C4 C5 C6 . . 117.4(3) C4 C5 H5A . . 108.0 C6 C5 H5A . . 108.0 C4 C5 H5B . . 108.0 C6 C5 H5B . . 108.0 H5A C5 H5B . . 107.2 N2 C6 C5 . . 114.0(3) N2 C6 H6A . . 108.8 C5 C6 H6A . . 108.8 N2 C6 H6B . . 108.8 C5 C6 H6B . . 108.8 H6A C6 H6B . . 107.6 N3 C7 C8 . . 112.4(2) N3 C7 H7A . . 109.1 C8 C7 H7A . . 109.1 N3 C7 H7B . . 109.1 C8 C7 H7B . . 109.1 H7A C7 H7B . . 107.9 C7 C8 C9 . . 115.8(3) C7 C8 H8A . . 108.3 C9 C8 H8A . . 108.3 C7 C8 H8B . . 108.3 C9 C8 H8B . . 108.3 H8A C8 H8B . . 107.4 C9 C9 C8 2_576 . 112.9(3) C9 C9 H9A 2_576 . 109.0 C8 C9 H9A . . 109.0 C9 C9 H9B 2_576 . 109.0 C8 C9 H9B . . 109.0 H9A C9 H9B . . 107.8 N4 C10 C11 . . 112.4(2) N4 C10 H10A . . 109.1 C11 C10 H10A . . 109.1 N4 C10 H10B . . 109.1 C11 C10 H10B . . 109.1 H10A C10 H10B . . 107.8 C10 C11 C12 . . 113.3(3) C10 C11 H11A . . 108.9 C12 C11 H11A . . 108.9 C10 C11 H11B . . 108.9 C12 C11 H11B . . 108.9 H11A C11 H11B . . 107.7 C12 C12 C11 2_565 . 114.8(3) C12 C12 H12A 2_565 . 108.6 C11 C12 H12A . . 108.6 C12 C12 H12B 2_565 . 108.6 C11 C12 H12B . . 108.6 H12A C12 H12B . . 107.6 C1 N1 H1NB . . 109.5 C1 N1 H1NA . . 109.5 H1NB N1 H1NA . . 109.5 C1 N1 H1NC . . 109.5 H1NB N1 H1NC . . 109.5 H1NA N1 H1NC . . 109.5 C6 N2 H2NA . . 109.5 C6 N2 H2NC . . 109.5 H2NA N2 H2NC . . 109.5 C6 N2 H2NB . . 109.5 H2NA N2 H2NB . . 109.5 H2NC N2 H2NB . . 109.5 C7 N3 H3NA . . 109.5 C7 N3 H3NB . . 109.5 H3NA N3 H3NB . . 109.5 C7 N3 H3NC . . 109.5 H3NA N3 H3NC . . 109.5 H3NB N3 H3NC . . 109.5 C10 N4 H4NA . . 109.5 C10 N4 H4NB . . 109.5 H4NA N4 H4NB . . 109.5 C10 N4 H4NC . . 109.5 H4NA N4 H4NC . . 109.5 H4NB N4 H4NC . . 109.5 F5 Si1 F1 . . 91.67(8) F5 Si1 F3 . . 91.24(10) F1 Si1 F3 . . 91.04(9) F5 Si1 F2 . . 179.11(10) F1 Si1 F2 . . 88.89(8) F3 Si1 F2 . . 89.43(9) F5 Si1 F4 . . 89.45(8) F1 Si1 F4 . . 178.85(9) F3 Si1 F4 . . 89.17(9) F2 Si1 F4 . . 89.98(8) F5 Si1 F6 . . 88.99(9) F1 Si1 F6 . . 89.33(8) F3 Si1 F6 . . 179.56(10) F2 Si1 F6 . . 90.33(9) F4 Si1 F6 . . 90.46(8) F9 Si2 F9 2_566 . 180.0 F9 Si2 F7 2_566 . 89.15(8) F9 Si2 F7 . . 90.85(8) F9 Si2 F7 2_566 2_566 90.85(8) F9 Si2 F7 . 2_566 89.15(8) F7 Si2 F7 . 2_566 180.0 F9 Si2 F8 2_566 . 90.78(9) F9 Si2 F8 . . 89.22(9) F7 Si2 F8 . . 89.29(8) F7 Si2 F8 2_566 . 90.71(8) F9 Si2 F8 2_566 2_566 89.22(9) F9 Si2 F8 . 2_566 90.78(9) F7 Si2 F8 . 2_566 90.71(8) F7 Si2 F8 2_566 2_566 89.29(8) F8 Si2 F8 . 2_566 180.0 F12 Si3 F12 . 2_575 180.0 F12 Si3 F11 . 2_575 89.08(8) F12 Si3 F11 2_575 2_575 90.92(8) F12 Si3 F11 . . 90.92(8) F12 Si3 F11 2_575 . 89.08(8) F11 Si3 F11 2_575 . 180.0000(10) F12 Si3 F10 . 2_575 89.24(9) F12 Si3 F10 2_575 2_575 90.76(9) F11 Si3 F10 2_575 2_575 90.66(9) F11 Si3 F10 . 2_575 89.34(9) F12 Si3 F10 . . 90.76(9) F12 Si3 F10 2_575 . 89.24(9) F11 Si3 F10 2_575 . 89.34(9) F11 Si3 F10 . . 90.66(9) F10 Si3 F10 2_575 . 180.00(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance C1 N1 . 1.466(4) C1 C2 . 1.500(4) C1 H1A . 0.9700 C1 H1B . 0.9700 C2 C3 . 1.498(5) C2 H2A . 0.9700 C2 H2B . 0.9700 C3 C4 . 1.527(5) C3 H3A . 0.9700 C3 H3B . 0.9700 C4 C5 . 1.467(5) C4 H4A . 0.9700 C4 H4B . 0.9700 C5 C6 . 1.499(5) C5 H5A . 0.9700 C5 H5B . 0.9700 C6 N2 . 1.466(4) C6 H6A . 0.9700 C6 H6B . 0.9700 C7 N3 . 1.478(3) C7 C8 . 1.495(4) C7 H7A . 0.9700 C7 H7B . 0.9700 C8 C9 . 1.507(4) C8 H8A . 0.9700 C8 H8B . 0.9700 C9 C9 2_576 1.506(5) C9 H9A . 0.9700 C9 H9B . 0.9700 C10 N4 . 1.465(3) C10 C11 . 1.489(4) C10 H10A . 0.9700 C10 H10B . 0.9700 C11 C12 . 1.508(4) C11 H11A . 0.9700 C11 H11B . 0.9700 C12 C12 2_565 1.499(6) C12 H12A . 0.9700 C12 H12B . 0.9700 N1 H1NB . 0.8900 N1 H1NA . 0.8900 N1 H1NC . 0.8900 N2 H2NA . 0.8900 N2 H2NC . 0.8900 N2 H2NB . 0.8900 N3 H3NA . 0.8900 N3 H3NB . 0.8900 N3 H3NC . 0.8900 N4 H4NA . 0.8900 N4 H4NB . 0.8900 N4 H4NC . 0.8900 F1 Si1 . 1.6794(15) F2 Si1 . 1.6837(15) F3 Si1 . 1.6798(17) F4 Si1 . 1.6868(15) F5 Si1 . 1.6677(16) F6 Si1 . 1.6915(16) F7 Si2 . 1.6848(14) F8 Si2 . 1.6858(16) F9 Si2 . 1.6741(15) F10 Si3 . 1.6848(17) F11 Si3 . 1.6830(14) F12 Si3 . 1.6759(14) Si2 F9 2_566 1.6741(15) Si2 F7 2_566 1.6849(14) Si2 F8 2_566 1.6858(16) Si3 F12 2_575 1.6760(14) Si3 F11 2_575 1.6830(14) Si3 F10 2_575 1.6848(17) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N2 H2NC F5 . 0.89 2.31 3.062(3) 141.6 N2 H2NC F6 . 0.89 2.27 3.063(3) 147.8 N2 H2NB F7 . 0.89 2.52 3.095(3) 123.3 N2 H2NB F8 . 0.89 2.03 2.917(3) 175.0 N3 H3NA F1 . 0.89 2.06 2.934(3) 168.6 N4 H4NA F8 . 0.89 2.34 3.095(3) 142.8 N4 H4NA F9 . 0.89 2.14 2.923(3) 146.1 N4 H4NC F6 . 0.89 2.00 2.885(3) 171.6 N1 H1NB F11 2_576 0.89 2.07 2.895(3) 154.6 N1 H1NA F10 2_676 0.89 2.01 2.869(3) 162.6 N1 H1NC F2 1_556 0.89 2.02 2.857(2) 155.3 N2 H2NA F7 2_666 0.89 2.02 2.906(3) 170.4 N3 H3NB F10 2_575 0.89 2.48 3.239(3) 143.6 N3 H3NB F12 . 0.89 2.13 2.907(2) 145.3 N3 H3NC F3 1_455 0.89 2.02 2.904(3) 170.3 N3 H3NC F4 1_455 0.89 2.44 3.034(3) 124.1 N4 H4NB F4 1_455 0.89 2.01 2.832(3) 153.7 N4 H4NB F5 1_455 0.89 2.51 3.086(3) 123.2