# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dai, Xuliang' _publ_contact_author_email xuliang.dai@ndsu.edu _publ_section_title ; New Coordination Chemistry of Si5Cl10 with Organocyanides ; _publ_requested_category FO loop_ _publ_author_name X.Dai K.Anderson D.Schulz P.Boudjouk # Attachment '- Si5Cl10(MeCN)2 and Si5Cl10(ArCN)2.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-04-09 at 13:53:03 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : dai12_0ma saint_dai12 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_Si5Cl10(MeCN)2 _database_code_depnum_ccdc_archive 'CCDC 776621' #TrackingRef '- Si5Cl10(MeCN)2 and Si5Cl10(ArCN)2.cif' _audit_creation_date 2010-04-09T13:53:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C4 H6 Cl10 N2 Si5' _chemical_formula_weight 577.06 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.904(8) _cell_length_b 13.186(8) _cell_length_c 12.688(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2159(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6022 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.45 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description bipyramide _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.56 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6371 _exptl_absorpt_correction_T_max 0.7457 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker 1K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_unetI/netI 0.021 _diffrn_reflns_number 14037 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.49 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 2720 _reflns_number_gt 2167 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0444P)^2^+0.7584P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2720 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.342 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.03147(4) 0.16749(4) 0.39611(4) 0.03729(14) Uani 1 1 d . . . Si2 Si 0.01924(4) 0.33670(4) 0.34021(5) 0.03993(15) Uani 1 1 d . . . Si3 Si 0 0.06250(6) 0.25 0.03592(17) Uani 1 2 d S . . Cl1 Cl -0.12285(5) -0.03045(4) 0.27774(5) 0.05410(16) Uani 1 1 d . . . Cl2 Cl 0.17437(4) 0.14055(5) 0.45816(4) 0.05784(17) Uani 1 1 d . . . Cl3 Cl -0.06987(5) 0.13962(5) 0.51583(4) 0.05726(17) Uani 1 1 d . . . Cl4 Cl -0.09020(5) 0.41333(5) 0.42382(6) 0.06459(19) Uani 1 1 d . . . Cl5 Cl 0.15370(5) 0.41229(5) 0.36974(6) 0.06427(19) Uani 1 1 d . . . N1 N 0.83194(15) 0.21729(17) 0.29208(16) 0.0551(5) Uani 1 1 d . . . C1 C 0.74754(18) 0.20284(17) 0.29475(17) 0.0480(5) Uani 1 1 d . . . C2 C 0.6386(2) 0.1830(3) 0.2950(4) 0.0980(13) Uani 1 1 d . . . H2A H 0.6167 0.1648 0.2252 0.147 Uiso 1 1 calc R . . H2B H 0.6021 0.2427 0.3173 0.147 Uiso 1 1 calc R . . H2C H 0.6239 0.1283 0.3425 0.147 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 0.0357(3) 0.0467(3) 0.0295(3) -0.0012(2) -0.00289(19) -0.0038(2) Si2 0.0353(3) 0.0402(3) 0.0443(3) -0.0077(2) 0.0096(2) -0.0056(2) Si3 0.0378(4) 0.0371(4) 0.0329(4) 0 -0.0069(3) 0 Cl1 0.0570(3) 0.0502(3) 0.0551(3) 0.0048(2) -0.0084(2) -0.0175(2) Cl2 0.0450(3) 0.0809(4) 0.0476(3) 0.0028(3) -0.0165(2) 0.0007(3) Cl3 0.0579(3) 0.0765(4) 0.0374(3) 0.0066(2) 0.0084(2) -0.0091(3) Cl4 0.0554(4) 0.0611(4) 0.0773(4) -0.0251(3) 0.0278(3) -0.0027(3) Cl5 0.0483(3) 0.0656(4) 0.0789(4) -0.0229(3) 0.0123(3) -0.0230(3) N1 0.0439(11) 0.0661(12) 0.0554(11) 0.0003(9) 0.0034(8) -0.0012(10) C1 0.0453(12) 0.0432(11) 0.0555(13) -0.0003(9) 0.0045(10) -0.0002(9) C2 0.0470(16) 0.077(2) 0.170(4) -0.019(2) 0.0114(19) -0.0109(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cl2 2.0362(13) . ? Si1 Cl3 2.0378(11) . ? Si1 Si2 2.3465(15) . ? Si1 Si3 2.3491(12) . ? Si2 Cl4 2.0349(11) . ? Si2 Cl5 2.0357(12) . ? Si2 Si2 2.3425(18) 3 ? Si3 Cl1 2.0345(11) . ? Si3 Cl1 2.0345(11) 3 ? Si3 Si1 2.3490(12) 3 ? N1 C1 1.106(3) . ? C1 C2 1.430(4) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Si1 Cl3 105.15(5) . . ? Cl2 Si1 Si2 110.10(3) . . ? Cl3 Si1 Si2 110.71(4) . . ? Cl2 Si1 Si3 111.03(4) . . ? Cl3 Si1 Si3 111.79(5) . . ? Si2 Si1 Si3 108.07(5) . . ? Cl4 Si2 Cl5 104.62(5) . . ? Cl4 Si2 Si2 111.25(5) . 3 ? Cl5 Si2 Si2 111.13(4) . 3 ? Cl4 Si2 Si1 111.18(4) . . ? Cl5 Si2 Si1 110.65(4) . . ? Si2 Si2 Si1 108.04(2) 3 . ? Cl1 Si3 Cl1 105.91(7) . 3 ? Cl1 Si3 Si1 110.91(3) . 3 ? Cl1 Si3 Si1 110.68(3) 3 3 ? Cl1 Si3 Si1 110.68(3) . . ? Cl1 Si3 Si1 110.91(3) 3 . ? Si1 Si3 Si1 107.78(6) 3 . ? N1 C1 C2 178.2(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? #===END data_Si5Cl10(ArCN)2 _database_code_depnum_ccdc_archive 'CCDC 776622' #TrackingRef '- Si5Cl10(MeCN)2 and Si5Cl10(ArCN)2.cif' _audit_creation_date 2010-04-12T10:34:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C16 H14 Cl10 N2 Si5' _chemical_formula_weight 729.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.995(3) _cell_length_b 17.434(5) _cell_length_c 17.646(5) _cell_angle_alpha 90 _cell_angle_beta 93.082(6) _cell_angle_gamma 90 _cell_volume 3070.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1633 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 21.89 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6519 _exptl_absorpt_correction_T_max 0.7452 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker 1K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_unetI/netI 0.134 _diffrn_reflns_number 17334 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.44 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 5655 _reflns_number_gt 2298 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5655 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.187 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.609 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si4 Si 0.4369(2) 0.45880(11) 0.70635(11) 0.0537(6) Uani 1 1 d . . . Cl02 Cl 0.3516(2) 0.35013(11) 0.53441(10) 0.0701(6) Uani 1 1 d . . . Cl03 Cl 0.7894(2) 0.46654(11) 0.77277(12) 0.0762(6) Uani 1 1 d . . . Si3 Si 0.4609(2) 0.23970(11) 0.70093(12) 0.0591(6) Uani 1 1 d . . . Si1 Si 0.3426(2) 0.34679(11) 0.65053(10) 0.0503(5) Uani 1 1 d . . . Si5 Si 0.6081(2) 0.41945(11) 0.79591(11) 0.0537(6) Uani 1 1 d . . . Cl07 Cl 0.1415(2) 0.33851(13) 0.66903(12) 0.0816(7) Uani 1 1 d . . . Si2 Si 0.6231(2) 0.28434(11) 0.79318(11) 0.0538(6) Uani 1 1 d . . . Cl09 Cl 0.5095(2) 0.52825(11) 0.62422(12) 0.0799(7) Uani 1 1 d . . . Cl1 Cl 0.5729(2) 0.45790(13) 0.90284(11) 0.0862(7) Uani 1 1 d . . . Cl10 Cl 0.2957(2) 0.52264(13) 0.75687(13) 0.0944(8) Uani 1 1 d . . . Cl6 Cl 0.5480(2) 0.17964(12) 0.61625(13) 0.0899(8) Uani 1 1 d . . . Cl4 Cl 0.5961(2) 0.23922(13) 0.89798(12) 0.0899(8) Uani 1 1 d . . . Cl5 Cl 0.3326(3) 0.16405(13) 0.74586(14) 0.1038(9) Uani 1 1 d . . . Cl8 Cl 0.8117(2) 0.25002(12) 0.76702(13) 0.0816(7) Uani 1 1 d . . . N1 N 0.6372(7) 0.3571(4) 0.6427(4) 0.0711(19) Uani 1 1 d . . . N2 N 0.3502(7) 0.3406(4) 0.8186(4) 0.083(2) Uani 1 1 d . . . C1 C 0.8012(7) 0.3755(4) 0.5375(4) 0.0505(18) Uani 1 1 d . . . C2 C 0.1827(7) 0.3643(4) 0.9217(4) 0.0503(18) Uani 1 1 d . . . C3 C 0.0509(8) 0.3743(4) 0.9038(5) 0.071(2) Uani 1 1 d . . . H3 H 0.0198 0.3722 0.8532 0.085 Uiso 1 1 calc R . . C4 C 0.7103(8) 0.3640(4) 0.5953(4) 0.0506(18) Uani 1 1 d . . . C5 C 0.0046(10) 0.3931(4) 1.0341(5) 0.075(3) Uani 1 1 d . . . C6 C 0.2293(8) 0.3701(4) 0.9969(4) 0.073(2) Uani 1 1 d . . . H6 H 0.3201 0.3645 1.0103 0.088 Uiso 1 1 calc R . . C7 C 0.8891(8) 0.3180(4) 0.5223(4) 0.068(2) Uani 1 1 d . . . H7 H 0.8912 0.273 0.5507 0.081 Uiso 1 1 calc R . . C8 C 0.2759(8) 0.3502(4) 0.8647(4) 0.060(2) Uani 1 1 d . . . C9 C -0.0939(10) 0.4082(5) 1.0943(5) 0.121(4) Uani 1 1 d . . . H9A H -0.047 0.4102 1.1431 0.181 Uiso 1 1 calc R . . H9B H -0.159 0.3677 1.0937 0.181 Uiso 1 1 calc R . . H9C H -0.1382 0.4562 1.0842 0.181 Uiso 1 1 calc R . . C10 C 0.7991(8) 0.4418(4) 0.4951(4) 0.071(2) Uani 1 1 d . . . H10 H 0.7388 0.4807 0.5053 0.086 Uiso 1 1 calc R . . C11 C -0.0390(8) 0.3878(5) 0.9597(6) 0.082(3) Uani 1 1 d . . . H11 H -0.1297 0.3933 0.9463 0.098 Uiso 1 1 calc R . . C12 C 0.9726(10) 0.3941(7) 0.4222(5) 0.092(3) Uani 1 1 d . . . C13 C 0.1394(10) 0.3841(5) 1.0512(4) 0.084(3) Uani 1 1 d . . . H13 H 0.1709 0.3876 1.1017 0.101 Uiso 1 1 calc R . . C14 C 0.8836(10) 0.4507(6) 0.4389(5) 0.094(3) Uani 1 1 d . . . H14 H 0.8817 0.496 0.411 0.113 Uiso 1 1 calc R . . C15 C 0.9742(9) 0.3279(6) 0.4645(6) 0.088(3) Uani 1 1 d . . . H15 H 1.034 0.289 0.4539 0.106 Uiso 1 1 calc R . . C16 C 1.0646(10) 0.4038(7) 0.3582(5) 0.151(5) Uani 1 1 d . . . H16A H 1.0495 0.453 0.3349 0.226 Uiso 1 1 calc R . . H16B H 1.0471 0.3641 0.3212 0.226 Uiso 1 1 calc R . . H16C H 1.156 0.4004 0.3776 0.226 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 Si4 0.0564(14) 0.0460(12) 0.0587(13) -0.0049(10) 0.0032(10) 0.0050(10) Cl02 0.0888(16) 0.0722(13) 0.0489(11) 0.0009(10) 0.0005(10) 0.0051(12) Cl03 0.0637(14) 0.0703(13) 0.0936(16) 0.0141(12) -0.0048(12) -0.0201(11) Si3 0.0617(15) 0.0475(12) 0.0670(15) 0.0068(11) -0.0072(11) -0.0057(11) Si1 0.0471(13) 0.0529(12) 0.0510(12) 0.0012(10) 0.0043(10) 0.0001(11) Si5 0.0538(14) 0.0518(12) 0.0552(13) -0.0039(10) 0.0014(11) -0.0059(11) Cl07 0.0465(13) 0.1147(18) 0.0833(15) 0.0027(13) -0.0014(10) -0.0086(12) Si2 0.0550(14) 0.0517(12) 0.0541(13) 0.0091(10) -0.0030(10) -0.0031(11) Cl09 0.0894(17) 0.0571(13) 0.0921(16) 0.0240(11) -0.0046(13) -0.0086(12) Cl1 0.0951(18) 0.0997(17) 0.0632(13) -0.0250(12) -0.0017(12) 0.0034(14) Cl10 0.0906(18) 0.0968(17) 0.0954(17) -0.0366(13) -0.0003(13) 0.0414(14) Cl6 0.1001(19) 0.0673(14) 0.0995(17) -0.0277(12) -0.0197(14) 0.0240(13) Cl4 0.1011(19) 0.0972(17) 0.0697(15) 0.0369(12) -0.0098(12) -0.0166(14) Cl5 0.104(2) 0.0870(17) 0.1166(19) 0.0438(14) -0.0241(15) -0.0481(15) Cl8 0.0636(15) 0.0792(15) 0.1010(17) -0.0047(12) -0.0071(12) 0.0177(12) N1 0.068(5) 0.082(5) 0.064(4) 0.003(4) 0.012(4) 0.002(4) N2 0.056(5) 0.128(6) 0.065(5) 0.004(4) 0.014(4) -0.007(4) C1 0.042(5) 0.065(5) 0.045(4) 0.005(4) 0.011(4) 0.002(4) C2 0.042(5) 0.059(5) 0.050(5) -0.001(4) 0.003(4) -0.004(4) C3 0.043(5) 0.089(6) 0.081(6) -0.008(5) 0.009(5) 0.004(4) C4 0.052(5) 0.051(5) 0.049(4) -0.001(4) 0.003(4) 0.001(4) C5 0.085(8) 0.055(5) 0.089(7) -0.017(5) 0.030(6) -0.013(5) C6 0.050(5) 0.107(7) 0.063(5) -0.008(5) -0.002(4) -0.006(5) C7 0.055(5) 0.072(5) 0.078(6) 0.000(5) 0.021(5) 0.006(5) C8 0.045(5) 0.073(5) 0.060(5) 0.007(4) 0.001(4) -0.009(4) C9 0.140(10) 0.093(7) 0.137(9) -0.037(6) 0.085(8) -0.017(7) C10 0.070(6) 0.071(6) 0.073(6) 0.016(5) 0.010(5) 0.024(5) C11 0.049(6) 0.090(6) 0.108(7) -0.010(6) 0.013(6) 0.005(5) C12 0.064(7) 0.150(10) 0.064(6) -0.024(7) 0.020(5) -0.022(7) C13 0.076(7) 0.133(8) 0.044(5) -0.019(5) 0.011(5) -0.008(6) C14 0.091(8) 0.127(9) 0.066(6) 0.036(6) 0.013(6) -0.020(7) C15 0.071(7) 0.098(7) 0.096(7) -0.035(6) 0.018(6) 0.000(6) C16 0.105(9) 0.274(15) 0.079(7) -0.019(8) 0.053(7) -0.057(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Si4 Cl10 2.040(3) . ? Si4 Cl09 2.051(3) . ? Si4 Si1 2.360(3) . ? Si4 Si5 2.368(3) . ? Cl02 Si1 2.057(3) . ? Cl03 Si5 2.050(3) . ? Si3 Cl5 2.030(3) . ? Si3 Cl6 2.056(3) . ? Si3 Si1 2.358(3) . ? Si3 Si2 2.366(3) . ? Si1 Cl07 2.058(3) . ? Si5 Cl1 2.051(3) . ? Si5 Si2 2.361(3) . ? Si2 Cl4 2.041(3) . ? Si2 Cl8 2.053(3) . ? N1 C4 1.146(8) . ? N2 C8 1.143(9) . ? C1 C7 1.368(9) . ? C1 C10 1.377(9) . ? C1 C4 1.416(9) . ? C2 C3 1.349(10) . ? C2 C6 1.386(9) . ? C2 C8 1.429(10) . ? C3 C11 1.390(10) . ? C3 H3 0.93 . ? C5 C11 1.363(11) . ? C5 C13 1.375(11) . ? C5 C9 1.509(10) . ? C6 C13 1.370(10) . ? C6 H6 0.93 . ? C7 C15 1.373(10) . ? C7 H7 0.93 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 C14 1.345(10) . ? C10 H10 0.93 . ? C11 H11 0.93 . ? C12 C14 1.372(12) . ? C12 C15 1.375(12) . ? C12 C16 1.504(11) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? 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 Cl10 Si4 Cl09 105.44(13) . . ? Cl10 Si4 Si1 111.35(13) . . ? Cl09 Si4 Si1 110.00(11) . . ? Cl10 Si4 Si5 111.01(12) . . ? Cl09 Si4 Si5 111.83(12) . . ? Si1 Si4 Si5 107.26(10) . . ? Cl5 Si3 Cl6 104.71(14) . . ? Cl5 Si3 Si1 110.31(13) . . ? Cl6 Si3 Si1 110.62(12) . . ? Cl5 Si3 Si2 111.63(12) . . ? Cl6 Si3 Si2 111.51(13) . . ? Si1 Si3 Si2 108.06(10) . . ? Cl02 Si1 Cl07 104.80(12) . . ? Cl02 Si1 Si3 110.51(11) . . ? Cl07 Si1 Si3 111.02(11) . . ? Cl02 Si1 Si4 110.76(11) . . ? Cl07 Si1 Si4 111.28(11) . . ? Si3 Si1 Si4 108.47(11) . . ? Cl03 Si5 Cl1 104.46(12) . . ? Cl03 Si5 Si2 109.74(12) . . ? Cl1 Si5 Si2 111.04(12) . . ? Cl03 Si5 Si4 111.46(11) . . ? Cl1 Si5 Si4 111.46(12) . . ? Si2 Si5 Si4 108.65(10) . . ? Cl4 Si2 Cl8 105.02(13) . . ? Cl4 Si2 Si5 110.76(12) . . ? Cl8 Si2 Si5 110.81(12) . . ? Cl4 Si2 Si3 112.19(12) . . ? Cl8 Si2 Si3 110.64(12) . . ? Si5 Si2 Si3 107.48(10) . . ? C7 C1 C10 119.9(7) . . ? C7 C1 C4 118.7(7) . . ? C10 C1 C4 121.3(7) . . ? C3 C2 C6 119.2(7) . . ? C3 C2 C8 121.5(7) . . ? C6 C2 C8 119.3(7) . . ? C2 C3 C11 121.1(8) . . ? C2 C3 H3 119.5 . . ? C11 C3 H3 119.5 . . ? N1 C4 C1 177.8(8) . . ? C11 C5 C13 117.6(8) . . ? C11 C5 C9 120.2(10) . . ? C13 C5 C9 122.2(9) . . ? C13 C6 C2 118.9(8) . . ? C13 C6 H6 120.5 . . ? C2 C6 H6 120.5 . . ? C1 C7 C15 118.9(8) . . ? C1 C7 H7 120.5 . . ? C15 C7 H7 120.5 . . ? N2 C8 C2 178.5(9) . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C1 120.4(8) . . ? C14 C10 H10 119.8 . . ? C1 C10 H10 119.8 . . ? C5 C11 C3 120.6(8) . . ? C5 C11 H11 119.7 . . ? C3 C11 H11 119.7 . . ? C14 C12 C15 118.4(8) . . ? C14 C12 C16 120.7(11) . . ? C15 C12 C16 120.9(11) . . ? C6 C13 C5 122.5(8) . . ? C6 C13 H13 118.7 . . ? C5 C13 H13 118.7 . . ? C10 C14 C12 121.0(9) . . ? C10 C14 H14 119.5 . . ? C12 C14 H14 119.5 . . ? C7 C15 C12 121.3(8) . . ? C7 C15 H15 119.4 . . ? C12 C15 H15 119.4 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? #===END