Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Smith, J. David' 'Eaborn, C.' 'Hill, Michael S.' 'Hitchcock, Peter B.' _publ_contact_author_name 'Dr J. David Smith' _publ_contact_author_address ; Chemistry, Physics and Environmental Science University of Sussex CPES University of Sussex Falmer Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'J.D.SMITH@SUSSEX.AC.UK' _publ_section_title ; Synthesis and structures of compounds of Groups 11 and 12 containing the Ligand C(SiMe3)2(SiMe2C5H4N-2) ; data_sep899 _database_code_CSD 177596 _audit_creation_date 1999-09-13T15:11:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C28 H56 Cu2 N2 Si6).(C7 H8)' _chemical_formula_sum 'C35 H64 Cu2 N2 Si6' _chemical_formula_weight 808.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.022(8) _cell_length_b 9.069(6) _cell_length_c 41.20(4) _cell_angle_alpha 90 _cell_angle_beta 90.47(3) _cell_angle_gamma 90 _cell_volume 8602(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 9.7 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION (not applied) #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.181 _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.891 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.23591E-1 _diffrn_orient_matrix_ub_12 0.92448E-1 _diffrn_orient_matrix_ub_13 0.1769E-2 _diffrn_orient_matrix_ub_21 -0.11315E-1 _diffrn_orient_matrix_ub_22 -0.28145E-1 _diffrn_orient_matrix_ub_23 0.22619E-1 _diffrn_orient_matrix_ub_31 0.34662E-1 _diffrn_orient_matrix_ub_32 0.53292E-1 _diffrn_orient_matrix_ub_33 0.8774E-2 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -7 _diffrn_standards_decay_corr_max 1 _diffrn_standards_decay_corr_min 0.904 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 3 -5 3 -3 -5 _diffrn_reflns_number 5370 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 22 _diffrn_reflns_theta_full 22 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5233 _reflns_number_gt 3361 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The data is undoubtedly affected by reflection overlap due to the long 'c' axis . It was necessary to put constraints on the ADPs (using DELU) . There are two molecules of toluene solvate, one on a 2-fold axis, and the other disordered about an inversion centre (H atoms omitted for atoms affected by disorder). 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^)+(0.1470P)^2^+187.7754P] 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 'riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5233 _refine_ls_number_parameters 373 _refine_ls_number_restraints 131 _refine_ls_R_factor_all 0.1462 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2780 _refine_ls_wR_factor_gt 0.2148 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.005 _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 Cu1 Cu 0.64656(6) 0.20855(15) 0.40998(4) 0.0247(5) Uani 1 1 d U . . Cu2 Cu 0.67386(6) 0.11473(15) 0.34616(4) 0.0240(5) Uani 1 1 d U . . Si1 Si 0.53465(14) 0.1915(3) 0.36574(9) 0.0239(8) Uani 1 1 d U . . Si2 Si 0.55233(15) 0.0284(4) 0.43211(9) 0.0285(9) Uani 1 1 d U . . Si3 Si 0.53634(16) 0.3704(4) 0.42964(10) 0.0332(10) Uani 1 1 d U . . Si4 Si 0.75785(14) 0.3643(3) 0.37028(9) 0.0233(8) Uani 1 1 d U . . Si5 Si 0.74299(15) 0.2842(4) 0.29757(9) 0.0279(9) Uani 1 1 d U . . Si6 Si 0.79905(14) 0.0568(4) 0.34527(9) 0.0262(9) Uani 1 1 d U . . N1 N 0.6097(4) -0.0194(10) 0.3404(3) 0.027(2) Uani 1 1 d U . . N2 N 0.7256(4) 0.2088(11) 0.4264(2) 0.027(2) Uani 1 1 d U . . C1 C 0.5627(5) 0.1988(12) 0.4080(3) 0.025(2) Uani 1 1 d U . . C2 C 0.4540(5) 0.2067(14) 0.3620(3) 0.035(3) Uani 1 1 d U . . H2A H 0.4412 0.3006 0.3713 0.052 Uiso 1 1 calc R . . H2B H 0.4358 0.1251 0.3737 0.052 Uiso 1 1 calc R . . H2C H 0.4426 0.2024 0.3391 0.052 Uiso 1 1 calc R . . C3 C 0.5630(5) 0.3285(12) 0.3358(3) 0.029(3) Uani 1 1 d U . . H3A H 0.6051 0.3164 0.3338 0.043 Uiso 1 1 calc R . . H3B H 0.5545 0.4286 0.3434 0.043 Uiso 1 1 calc R . . H3C H 0.5444 0.3123 0.3147 0.043 Uiso 1 1 calc R . . C4 C 0.5536(5) 0.0073(12) 0.3468(3) 0.019(2) Uani 1 1 d U . . C5 C 0.5124(5) -0.1005(13) 0.3392(3) 0.030(3) Uani 1 1 d U . . H5 H 0.4729 -0.0824 0.3443 0.036 Uiso 1 1 calc R . . C6 C 0.5268(6) -0.2323(14) 0.3246(3) 0.035(3) Uani 1 1 d U . . H6 H 0.4982 -0.3047 0.3198 0.042 Uiso 1 1 calc R . . C7 C 0.5843(6) -0.2546(13) 0.3174(4) 0.036(3) Uani 1 1 d U . . H7 H 0.5964 -0.3422 0.3068 0.043 Uiso 1 1 calc R . . C8 C 0.6238(5) -0.1490(13) 0.3258(3) 0.029(3) Uani 1 1 d U . . H8 H 0.6635 -0.1669 0.3211 0.035 Uiso 1 1 calc R . . C9 C 0.6036(5) -0.1256(13) 0.4199(3) 0.034(3) Uani 1 1 d U . . H9A H 0.6438 -0.0935 0.4232 0.051 Uiso 1 1 calc R . . H9B H 0.5973 -0.1498 0.3969 0.051 Uiso 1 1 calc R . . H9C H 0.5961 -0.2130 0.4332 0.051 Uiso 1 1 calc R . . C10 C 0.4772(5) -0.0545(15) 0.4296(3) 0.037(3) Uani 1 1 d U . . H10A H 0.4680 -0.0796 0.4070 0.056 Uiso 1 1 calc R . . H10B H 0.4487 0.0169 0.4376 0.056 Uiso 1 1 calc R . . H10C H 0.4757 -0.1439 0.4429 0.056 Uiso 1 1 calc R . . C11 C 0.5672(7) 0.0550(17) 0.4766(3) 0.048(4) Uani 1 1 d U . . H11A H 0.5411 0.1308 0.4851 0.072 Uiso 1 1 calc R . . H11B H 0.6076 0.0862 0.4798 0.072 Uiso 1 1 calc R . . H11C H 0.5606 -0.0381 0.4881 0.072 Uiso 1 1 calc R . . C12 C 0.4636(6) 0.3437(17) 0.4502(4) 0.051(4) Uani 1 1 d U . . H12A H 0.4336 0.3247 0.4338 0.077 Uiso 1 1 calc R . . H12B H 0.4537 0.4329 0.4624 0.077 Uiso 1 1 calc R . . H12C H 0.4660 0.2596 0.4651 0.077 Uiso 1 1 calc R . . C13 C 0.5879(7) 0.4365(16) 0.4621(3) 0.046(3) Uani 1 1 d U . . H13A H 0.5708 0.5207 0.4734 0.069 Uiso 1 1 calc R . . H13B H 0.6246 0.4667 0.4521 0.069 Uiso 1 1 calc R . . H13C H 0.5953 0.3566 0.4776 0.069 Uiso 1 1 calc R . . C14 C 0.5254(6) 0.5319(13) 0.4017(4) 0.039(3) Uani 1 1 d U . . H14A H 0.4965 0.5065 0.3850 0.058 Uiso 1 1 calc R . . H14B H 0.5623 0.5567 0.3913 0.058 Uiso 1 1 calc R . . H14C H 0.5116 0.6168 0.4142 0.058 Uiso 1 1 calc R . . C15 C 0.7483(5) 0.2156(12) 0.3406(3) 0.022(2) Uani 1 1 d U . . C16 C 0.8224(5) 0.4836(14) 0.3634(4) 0.046(4) Uani 1 1 d U . . H16A H 0.8188 0.5317 0.3422 0.069 Uiso 1 1 calc R . . H16B H 0.8577 0.4231 0.3639 0.069 Uiso 1 1 calc R . . H16C H 0.8247 0.5588 0.3804 0.069 Uiso 1 1 calc R . . C17 C 0.6966(5) 0.4990(13) 0.3769(3) 0.031(3) Uani 1 1 d U . . H17A H 0.6620 0.4457 0.3841 0.047 Uiso 1 1 calc R . . H17B H 0.6878 0.5503 0.3565 0.047 Uiso 1 1 calc R . . H17C H 0.7082 0.5711 0.3934 0.047 Uiso 1 1 calc R . . C18 C 0.7709(5) 0.2784(12) 0.4123(3) 0.024(2) Uani 1 1 d U . . C19 C 0.8243(6) 0.2786(16) 0.4283(3) 0.037(3) Uani 1 1 d U . . H19 H 0.8555 0.3323 0.4191 0.044 Uiso 1 1 calc R . . C20 C 0.8335(6) 0.2046(18) 0.4567(4) 0.046(4) Uani 1 1 d U . . H20 H 0.8706 0.2036 0.4669 0.055 Uiso 1 1 calc R . . C21 C 0.7875(6) 0.1323(17) 0.4698(4) 0.045(3) Uani 1 1 d U . . H21 H 0.7922 0.0792 0.4895 0.054 Uiso 1 1 calc R . . C22 C 0.7347(6) 0.1360(15) 0.4545(3) 0.034(3) Uani 1 1 d U . . H22 H 0.7030 0.0855 0.4641 0.041 Uiso 1 1 calc R . . C23 C 0.6963(6) 0.1652(15) 0.2712(3) 0.040(3) Uani 1 1 d U . . H23A H 0.6567 0.1630 0.2798 0.060 Uiso 1 1 calc R . . H23B H 0.7121 0.0649 0.2708 0.060 Uiso 1 1 calc R . . H23C H 0.6955 0.2052 0.2491 0.060 Uiso 1 1 calc R . . C24 C 0.8158(6) 0.2998(16) 0.2771(4) 0.043(4) Uani 1 1 d U . . H24A H 0.8346 0.2028 0.2767 0.064 Uiso 1 1 calc R . . H24B H 0.8404 0.3694 0.2892 0.064 Uiso 1 1 calc R . . H24C H 0.8103 0.3353 0.2548 0.064 Uiso 1 1 calc R . . C25 C 0.7097(6) 0.4720(14) 0.2936(3) 0.036(3) Uani 1 1 d U . . H25A H 0.7330 0.5435 0.3059 0.054 Uiso 1 1 calc R . . H25B H 0.6701 0.4702 0.3021 0.054 Uiso 1 1 calc R . . H25C H 0.7085 0.5006 0.2706 0.054 Uiso 1 1 calc R . . C26 C 0.7865(6) -0.0644(14) 0.3813(4) 0.041(3) Uani 1 1 d U . . H26A H 0.7474 -0.1069 0.3799 0.061 Uiso 1 1 calc R . . H26B H 0.7902 -0.0060 0.4012 0.061 Uiso 1 1 calc R . . H26C H 0.8154 -0.1439 0.3816 0.061 Uiso 1 1 calc R . . C27 C 0.7972(5) -0.0787(14) 0.3101(3) 0.032(3) Uani 1 1 d U . . H27A H 0.8075 -0.0275 0.2901 0.048 Uiso 1 1 calc R . . H27B H 0.7581 -0.1202 0.3080 0.048 Uiso 1 1 calc R . . H27C H 0.8251 -0.1583 0.3143 0.048 Uiso 1 1 calc R . . C28 C 0.8777(5) 0.1157(15) 0.3482(4) 0.037(3) Uani 1 1 d U . . H28A H 0.8831 0.1800 0.3671 0.056 Uiso 1 1 calc R . . H28B H 0.8883 0.1692 0.3284 0.056 Uiso 1 1 calc R . . H28C H 0.9024 0.0283 0.3505 0.056 Uiso 1 1 calc R . . C29 C 0.7788(15) 0.700(4) 0.4702(8) 0.147(11) Uiso 1 1 d U . . C30 C 0.7159(10) 0.727(2) 0.4786(6) 0.087(6) Uiso 1 1 d U . . H30 H 0.6918 0.7070 0.4602 0.104 Uiso 1 1 calc R . . C31 C 0.6870(15) 0.765(4) 0.5008(8) 0.151(12) Uiso 1 1 d U . . H31 H 0.6458 0.7714 0.4999 0.181 Uiso 1 1 calc R . . C32 C 0.8127(14) 0.668(4) 0.4576(8) 0.047(8) Uiso 0.50 1 d PU . . C33 C 0.5000 0.222(4) 0.2500 0.088(9) Uiso 1 2 d SU . . C34 C 0.5444(10) 0.303(3) 0.2386(5) 0.092(7) Uiso 1 1 d U . . H34 H 0.5767 0.2523 0.2296 0.110 Uiso 1 1 calc R . . C35 C 0.5454(10) 0.449(3) 0.2392(5) 0.094(7) Uiso 1 1 d U . . H35 H 0.5788 0.5010 0.2319 0.112 Uiso 1 1 calc R . . C36 C 0.5000 0.523(5) 0.2500 0.116(12) Uiso 1 2 d SU . . H36 H 0.5000 0.6278 0.2500 0.139 Uiso 1 2 calc SR . . C37 C 0.5000 0.050(8) 0.2500 0.25(3) Uiso 1 2 d SU . . H37A H 0.5332 0.0141 0.2627 0.376 Uiso 0.25 1 calc PR . . H37B H 0.5029 0.0141 0.2276 0.376 Uiso 0.25 1 calc PR . . H37C H 0.4639 0.0141 0.2596 0.376 Uiso 0.25 1 calc PR . . H37D H 0.4668 0.0141 0.2373 0.376 Uiso 0.25 1 calc PR . . H37E H 0.4971 0.0141 0.2724 0.376 Uiso 0.25 1 calc PR . . H37F H 0.5361 0.0141 0.2404 0.376 Uiso 0.25 1 calc PR . . 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 Cu1 0.0261(9) 0.0121(8) 0.0360(10) 0.0005(7) 0.0065(7) -0.0045(7) Cu2 0.0235(8) 0.0090(8) 0.0396(10) -0.0003(7) 0.0074(7) -0.0042(6) Si1 0.0244(18) 0.0061(16) 0.041(2) -0.0018(15) 0.0055(15) -0.0017(14) Si2 0.036(2) 0.0151(18) 0.035(2) 0.0034(16) 0.0141(17) -0.0074(16) Si3 0.035(2) 0.0166(18) 0.048(3) -0.0080(18) 0.0121(18) -0.0037(17) Si4 0.0255(18) 0.0065(16) 0.038(2) 0.0000(15) 0.0104(15) -0.0056(14) Si5 0.036(2) 0.0154(18) 0.033(2) 0.0058(16) 0.0131(16) 0.0041(16) Si6 0.0245(18) 0.0103(17) 0.044(2) 0.0033(16) 0.0097(16) 0.0023(14) N1 0.024(4) 0.007(5) 0.050(7) 0.002(4) 0.009(5) -0.007(4) N2 0.035(4) 0.015(5) 0.032(5) 0.001(4) 0.010(4) -0.002(4) C1 0.038(5) 0.007(4) 0.031(5) -0.002(4) 0.012(4) -0.003(5) C2 0.027(6) 0.022(7) 0.056(9) -0.006(7) 0.004(5) 0.002(5) C3 0.039(7) 0.007(5) 0.041(7) 0.000(5) 0.008(6) -0.004(5) C4 0.027(5) 0.010(5) 0.021(6) 0.003(4) 0.006(5) 0.001(4) C5 0.019(6) 0.020(6) 0.050(9) -0.004(6) 0.011(6) -0.003(5) C6 0.034(6) 0.018(6) 0.055(9) -0.005(6) 0.005(6) -0.012(6) C7 0.037(6) 0.009(6) 0.061(10) -0.012(6) 0.007(7) 0.006(5) C8 0.027(6) 0.018(6) 0.043(8) -0.003(5) 0.013(6) 0.001(4) C9 0.035(7) 0.013(5) 0.053(9) 0.002(6) -0.001(6) -0.002(5) C10 0.040(6) 0.030(8) 0.042(8) 0.007(7) 0.014(6) -0.010(5) C11 0.066(10) 0.040(9) 0.039(6) 0.002(6) 0.010(6) -0.015(8) C12 0.051(7) 0.039(9) 0.064(11) -0.008(7) 0.029(7) -0.001(7) C13 0.069(9) 0.031(8) 0.038(8) -0.019(6) 0.014(6) -0.003(7) C14 0.050(9) 0.010(6) 0.056(9) -0.007(5) 0.007(6) 0.005(6) C15 0.020(5) 0.009(5) 0.036(5) 0.001(4) 0.005(4) -0.002(3) C16 0.031(7) 0.016(7) 0.091(12) 0.009(7) 0.012(7) -0.012(5) C17 0.039(7) 0.005(6) 0.049(9) -0.006(5) 0.010(6) -0.001(5) C18 0.027(5) 0.007(6) 0.039(6) -0.010(5) 0.005(4) -0.005(5) C19 0.030(6) 0.040(8) 0.041(7) -0.009(6) 0.002(5) -0.002(6) C20 0.033(7) 0.062(11) 0.043(8) 0.002(7) -0.005(6) 0.005(7) C21 0.042(7) 0.045(9) 0.049(9) -0.001(7) -0.003(6) 0.008(7) C22 0.037(6) 0.031(8) 0.035(7) 0.001(6) 0.008(5) -0.007(6) C23 0.051(8) 0.032(7) 0.036(8) -0.002(6) 0.001(6) 0.004(6) C24 0.042(7) 0.030(8) 0.057(9) 0.006(7) 0.018(6) 0.009(6) C25 0.039(8) 0.021(6) 0.047(9) 0.007(6) 0.005(6) 0.011(6) C26 0.045(8) 0.021(7) 0.056(8) 0.012(6) 0.012(6) 0.013(6) C27 0.026(7) 0.022(7) 0.049(7) -0.002(5) 0.006(6) 0.006(5) C28 0.028(5) 0.029(8) 0.054(9) -0.005(7) 0.006(6) 0.005(5) _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 Cu1 C1 1.934(12) . ? Cu1 N2 1.936(10) . ? Cu1 Cu2 2.839(3) . ? Cu1 Si2 2.870(4) . ? Cu2 N1 1.927(9) . ? Cu2 C15 1.957(11) . ? Cu2 Si6 2.930(4) . ? Si1 C1 1.854(13) . ? Si1 C2 1.867(12) . ? Si1 C3 1.872(12) . ? Si1 C4 1.897(11) . ? Si2 C1 1.853(12) . ? Si2 C11 1.877(15) . ? Si2 C10 1.889(13) . ? Si2 C9 1.899(13) . ? Si3 C14 1.878(14) . ? Si3 C13 1.879(15) . ? Si3 C1 1.895(12) . ? Si3 C12 1.899(14) . ? Si4 C15 1.833(12) . ? Si4 C16 1.863(12) . ? Si4 C17 1.887(12) . ? Si4 C18 1.919(13) . ? Si5 C23 1.867(14) . ? Si5 C25 1.875(12) . ? Si5 C15 1.881(13) . ? Si5 C24 1.888(13) . ? Si6 C15 1.864(12) . ? Si6 C26 1.869(14) . ? Si6 C28 1.891(12) . ? Si6 C27 1.899(13) . ? N1 C4 1.342(14) . ? N1 C8 1.361(15) . ? N2 C22 1.350(16) . ? N2 C18 1.354(15) . ? C4 C5 1.395(16) . ? C5 C6 1.379(18) . ? C6 C7 1.374(18) . ? C7 C8 1.362(17) . ? C18 C19 1.389(17) . ? C19 C20 1.36(2) . ? C20 C21 1.36(2) . ? C21 C22 1.364(18) . ? C29 C32 0.98(4) . ? C29 C31 1.46(4) 7_666 ? C29 C30 1.51(4) . ? C30 C31 1.19(3) . ? C31 C29 1.46(4) 7_666 ? C31 C32 1.82(5) 7_666 ? C32 C31 1.82(5) 7_666 ? C33 C34 1.34(3) 2_655 ? C33 C34 1.34(3) . ? C33 C37 1.56(7) . ? C34 C35 1.33(3) . ? C35 C36 1.32(3) . ? C36 C35 1.32(3) 2_655 ? 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 C1 Cu1 N2 161.8(5) . . ? C1 Cu1 Cu2 100.2(4) . . ? N2 Cu1 Cu2 96.3(3) . . ? C1 Cu1 Si2 39.7(4) . . ? N2 Cu1 Si2 126.9(3) . . ? Cu2 Cu1 Si2 107.29(10) . . ? N1 Cu2 C15 162.1(5) . . ? N1 Cu2 Cu1 97.3(3) . . ? C15 Cu2 Cu1 99.8(4) . . ? N1 Cu2 Si6 129.7(3) . . ? C15 Cu2 Si6 38.8(3) . . ? Cu1 Cu2 Si6 106.89(10) . . ? C1 Si1 C2 114.4(6) . . ? C1 Si1 C3 118.3(6) . . ? C2 Si1 C3 104.4(6) . . ? C1 Si1 C4 109.8(5) . . ? C2 Si1 C4 105.3(6) . . ? C3 Si1 C4 103.3(5) . . ? C1 Si2 C11 113.1(6) . . ? C1 Si2 C10 115.1(6) . . ? C11 Si2 C10 105.3(6) . . ? C1 Si2 C9 112.9(6) . . ? C11 Si2 C9 104.2(7) . . ? C10 Si2 C9 105.3(6) . . ? C1 Si2 Cu1 41.8(4) . . ? C11 Si2 Cu1 96.0(5) . . ? C10 Si2 Cu1 154.6(5) . . ? C9 Si2 Cu1 82.0(4) . . ? C14 Si3 C13 105.6(7) . . ? C14 Si3 C1 113.2(6) . . ? C13 Si3 C1 113.2(6) . . ? C14 Si3 C12 105.0(7) . . ? C13 Si3 C12 106.1(7) . . ? C1 Si3 C12 113.1(6) . . ? C15 Si4 C16 114.6(6) . . ? C15 Si4 C17 119.1(6) . . ? C16 Si4 C17 104.1(6) . . ? C15 Si4 C18 108.7(5) . . ? C16 Si4 C18 104.7(6) . . ? C17 Si4 C18 104.2(6) . . ? C23 Si5 C25 103.9(6) . . ? C23 Si5 C15 112.9(6) . . ? C25 Si5 C15 114.0(6) . . ? C23 Si5 C24 107.0(7) . . ? C25 Si5 C24 104.9(6) . . ? C15 Si5 C24 113.2(6) . . ? C15 Si6 C26 115.8(6) . . ? C15 Si6 C28 112.8(6) . . ? C26 Si6 C28 105.7(7) . . ? C15 Si6 C27 114.2(6) . . ? C26 Si6 C27 102.8(6) . . ? C28 Si6 C27 104.3(6) . . ? C15 Si6 Cu2 41.1(3) . . ? C26 Si6 Cu2 86.4(4) . . ? C28 Si6 Cu2 152.9(4) . . ? C27 Si6 Cu2 96.3(4) . . ? C4 N1 C8 118.3(10) . . ? C4 N1 Cu2 126.9(8) . . ? C8 N1 Cu2 114.5(8) . . ? C22 N2 C18 118.9(11) . . ? C22 N2 Cu1 115.9(8) . . ? C18 N2 Cu1 125.2(8) . . ? Si2 C1 Si1 115.4(6) . . ? Si2 C1 Si3 113.0(6) . . ? Si1 C1 Si3 111.1(6) . . ? Si2 C1 Cu1 98.5(6) . . ? Si1 C1 Cu1 112.4(6) . . ? Si3 C1 Cu1 105.4(6) . . ? N1 C4 C5 118.9(10) . . ? N1 C4 Si1 117.7(8) . . ? C5 C4 Si1 123.5(9) . . ? C6 C5 C4 122.7(11) . . ? C7 C6 C5 117.1(12) . . ? C8 C7 C6 118.9(12) . . ? N1 C8 C7 124.0(11) . . ? Si4 C15 Si6 115.3(6) . . ? Si4 C15 Si5 113.1(6) . . ? Si6 C15 Si5 112.9(6) . . ? Si4 C15 Cu2 111.4(6) . . ? Si6 C15 Cu2 100.1(5) . . ? Si5 C15 Cu2 102.4(6) . . ? N2 C18 C19 118.6(12) . . ? N2 C18 Si4 117.4(9) . . ? C19 C18 Si4 124.0(10) . . ? C20 C19 C18 122.5(13) . . ? C21 C20 C19 117.5(13) . . ? C20 C21 C22 120.0(14) . . ? N2 C22 C21 122.6(13) . . ? C32 C29 C31 94(4) . 7_666 ? C32 C29 C30 159(4) . . ? C31 C29 C30 107(3) 7_666 . ? C31 C30 C29 140(3) . . ? C30 C31 C29 113(3) . 7_666 ? C30 C31 C32 146(3) . 7_666 ? C29 C31 C32 32.6(18) 7_666 7_666 ? C29 C32 C31 53(3) . 7_666 ? C34 C33 C34 114(3) 2_655 . ? C34 C33 C37 122.9(16) 2_655 . ? C34 C33 C37 122.9(17) . . ? C35 C34 C33 123(3) . . ? C36 C35 C34 120(3) . . ? C35 C36 C35 119(4) 2_655 . ? #===END data_ce-jds-3 _database_code_CSD 177597 _audit_creation_date 2000-01-21T17:19:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Au(C(SiMe3)2(SiMe2C5H4N)}2]' _chemical_formula_moiety 'C26 H56 Au2 N2 Si6' _chemical_formula_structural 'C26 H56 AU2 N2 SI6' _chemical_formula_sum 'C26 H56 Au2 N2 Si6' _chemical_formula_weight 959.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 20.7045(6) _cell_length_b 11.9894(3) _cell_length_c 32.9397(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8176.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 60337 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3236 _exptl_absorpt_correction_T_max 0.4169 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 27361 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.53 _diffrn_reflns_theta_max 21.96 _diffrn_reflns_theta_full 21.96 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 9715 _reflns_number_gt 8892 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The crystals were all small and poorly formed with intergrown habit. One crystal was selected that appeared to be cleaner than the rest and was used for data collection. A few weak reflections indicating a double length b axis were ignored as structure solution in the larger cell simply gave molecules with a repeat of 0.5 along the b axis. There appears to be a small amount of an alternative molecular arrangement related by a mirror reflection perpendicular to the b axis for which only the Au positions were identifiable. Because of this problem the C and N atoms had to be left isotropic to stop them going non-positive-definite. 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^)+(0.0353P)^2^+451.1801P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9715 _refine_ls_number_parameters 403 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.1809 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.13 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.278(18) _refine_diff_density_max 1.963 _refine_diff_density_min -1.991 _refine_diff_density_rms 0.266 #----------------------------------------------------------------------------# # 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' Au Au -2.0133 8.8022 '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' 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 Au1 Au 0.29176(6) 0.68529(9) 0.41804(3) 0.0245(3) Uani 0.9513(19) 1 d P A 1 Au2 Au 0.43205(6) 0.62670(9) 0.39605(3) 0.0218(3) Uani 0.9513(19) 1 d P A 1 Si1 Si 0.3915(4) 0.7827(6) 0.4862(2) 0.0145(17) Uani 0.9513(19) 1 d P A 1 Si2 Si 0.2418(4) 0.7713(7) 0.5023(2) 0.0205(18) Uani 0.9513(19) 1 d P A 1 Si3 Si 0.2965(4) 0.9377(6) 0.4377(2) 0.0192(18) Uani 0.9513(19) 1 d P A 1 Si4 Si 0.3406(4) 0.4057(6) 0.3899(2) 0.0185(17) Uani 0.9513(19) 1 d P A 1 Si5 Si 0.4247(4) 0.4909(6) 0.3175(2) 0.0183(19) Uani 0.9513(19) 1 d P A 1 Si6 Si 0.4910(4) 0.3876(9) 0.3953(3) 0.041(2) Uani 0.9513(19) 1 d P A 1 N1 N 0.4645(10) 0.7898(17) 0.4128(6) 0.016(5) Uiso 0.9513(19) 1 d P A 1 N2 N 0.2577(11) 0.5869(18) 0.3704(6) 0.020(5) Uiso 0.9513(19) 1 d P A 1 C1 C 0.3076(12) 0.797(2) 0.4639(7) 0.011(6) Uiso 0.9513(19) 1 d P A 1 C2 C 0.4052(15) 0.860(2) 0.5358(8) 0.025(7) Uiso 0.9513(19) 1 d P A 1 H2A H 0.3915 0.9375 0.5328 0.038 Uiso 0.9513(19) 1 calc PR A 1 H2B H 0.4512 0.8573 0.5428 0.038 Uiso 0.9513(19) 1 calc PR A 1 H2C H 0.38 0.8241 0.5574 0.038 Uiso 0.9513(19) 1 calc PR A 1 C3 C 0.4187(14) 0.637(2) 0.4971(8) 0.018(6) Uiso 0.9513(19) 1 d P A 1 H3A H 0.4623 0.6389 0.5087 0.027 Uiso 0.9513(19) 1 calc PR A 1 H3B H 0.4193 0.5941 0.4718 0.027 Uiso 0.9513(19) 1 calc PR A 1 H3C H 0.389 0.6022 0.5164 0.027 Uiso 0.9513(19) 1 calc PR A 1 C4 C 0.4532(14) 0.841(2) 0.4479(8) 0.020(6) Uiso 0.9513(19) 1 d P A 1 C5 C 0.4880(16) 0.943(3) 0.4586(10) 0.036(8) Uiso 0.9513(19) 1 d P A 1 H5 H 0.4847 0.9739 0.4851 0.043 Uiso 0.9513(19) 1 calc PR A 1 C6 C 0.5233(17) 0.991(3) 0.4312(10) 0.033(8) Uiso 0.9513(19) 1 d P A 1 H6 H 0.5394 1.0645 0.4357 0.04 Uiso 0.9513(19) 1 calc PR A 1 C7 C 0.5381(17) 0.934(3) 0.3942(11) 0.046(8) Uiso 0.9513(19) 1 d P A 1 H7 H 0.5687 0.9639 0.3757 0.055 Uiso 0.9513(19) 1 calc PR A 1 C8 C 0.5080(15) 0.835(3) 0.3856(9) 0.034(8) Uiso 0.9513(19) 1 d P A 1 H8 H 0.517 0.798 0.3608 0.041 Uiso 0.9513(19) 1 calc PR A 1 C9 C 0.2638(15) 0.655(2) 0.5382(9) 0.028(7) Uiso 0.9513(19) 1 d P A 1 H9A H 0.2287 0.6439 0.5577 0.043 Uiso 0.9513(19) 1 calc PR A 1 H9B H 0.3035 0.6746 0.5528 0.043 Uiso 0.9513(19) 1 calc PR A 1 H9C H 0.2707 0.5861 0.5228 0.043 Uiso 0.9513(19) 1 calc PR A 1 C10 C 0.2235(16) 0.899(3) 0.5360(10) 0.036(8) Uiso 0.9513(19) 1 d P A 1 H10A H 0.1889 0.8801 0.5551 0.054 Uiso 0.9513(19) 1 calc PR A 1 H10B H 0.2097 0.9614 0.5189 0.054 Uiso 0.9513(19) 1 calc PR A 1 H10C H 0.2624 0.9199 0.551 0.054 Uiso 0.9513(19) 1 calc PR A 1 C11 C 0.1612(13) 0.729(2) 0.4769(8) 0.015(6) Uiso 0.9513(19) 1 d P A 1 H11A H 0.1284 0.7171 0.4979 0.023 Uiso 0.9513(19) 1 calc PR A 1 H11B H 0.1673 0.6607 0.4613 0.023 Uiso 0.9513(19) 1 calc PR A 1 H11C H 0.147 0.7892 0.4587 0.023 Uiso 0.9513(19) 1 calc PR A 1 C12 C 0.2095(16) 0.960(3) 0.4249(10) 0.032(7) Uiso 0.9513(19) 1 d P A 1 H12A H 0.1836 0.9572 0.4498 0.048 Uiso 0.9513(19) 1 calc PR A 1 H12B H 0.195 0.9022 0.4061 0.048 Uiso 0.9513(19) 1 calc PR A 1 H12C H 0.2042 1.0336 0.4122 0.048 Uiso 0.9513(19) 1 calc PR A 1 C13 C 0.3395(14) 0.945(2) 0.3892(8) 0.023(7) Uiso 0.9513(19) 1 d P A 1 H13A H 0.3857 0.9329 0.3938 0.035 Uiso 0.9513(19) 1 calc PR A 1 H13B H 0.333 1.0189 0.3771 0.035 Uiso 0.9513(19) 1 calc PR A 1 H13C H 0.3229 0.8876 0.3709 0.035 Uiso 0.9513(19) 1 calc PR A 1 C14 C 0.3217(14) 1.063(2) 0.4681(8) 0.023(7) Uiso 0.9513(19) 1 d P A 1 H14A H 0.2991 1.0628 0.4943 0.035 Uiso 0.9513(19) 1 calc PR A 1 H14B H 0.3106 1.1313 0.4532 0.035 Uiso 0.9513(19) 1 calc PR A 1 H14C H 0.3684 1.0609 0.4728 0.035 Uiso 0.9513(19) 1 calc PR A 1 C15 C 0.4199(14) 0.467(2) 0.3740(8) 0.018(6) Uiso 0.9513(19) 1 d P A 1 C16 C 0.3194(16) 0.415(3) 0.4440(9) 0.032(8) Uiso 0.9513(19) 1 d P A 1 H16A H 0.3527 0.3781 0.4603 0.047 Uiso 0.9513(19) 1 calc PR A 1 H16B H 0.2777 0.3787 0.4486 0.047 Uiso 0.9513(19) 1 calc PR A 1 H16C H 0.3164 0.4938 0.452 0.047 Uiso 0.9513(19) 1 calc PR A 1 C17 C 0.3340(13) 0.257(2) 0.3762(8) 0.014(6) Uiso 0.9513(19) 1 d P A 1 H17A H 0.3672 0.2146 0.3907 0.021 Uiso 0.9513(19) 1 calc PR A 1 H17B H 0.3402 0.2485 0.3469 0.021 Uiso 0.9513(19) 1 calc PR A 1 H17C H 0.2912 0.2294 0.3838 0.021 Uiso 0.9513(19) 1 calc PR A 1 C18 C 0.2744(15) 0.478(2) 0.3601(9) 0.018(7) Uiso 0.9513(19) 1 d P A 1 C19 C 0.2388(16) 0.425(3) 0.3311(9) 0.034(8) Uiso 0.9513(19) 1 d P A 1 H19 H 0.2473 0.3481 0.3264 0.04 Uiso 0.9513(19) 1 calc PR A 1 C20 C 0.1896(17) 0.477(3) 0.3074(10) 0.035(8) Uiso 0.9513(19) 1 d P A 1 H20 H 0.1659 0.4371 0.2874 0.043 Uiso 0.9513(19) 1 calc PR A 1 C21 C 0.1791(14) 0.582(2) 0.3147(8) 0.024(7) Uiso 0.9513(19) 1 d P A 1 H21 H 0.1485 0.6216 0.2988 0.029 Uiso 0.9513(19) 1 calc PR A 1 C22 C 0.2136(17) 0.640(3) 0.3469(10) 0.040(8) Uiso 0.9513(19) 1 d P A 1 H22 H 0.205 0.7163 0.3516 0.048 Uiso 0.9513(19) 1 calc PR A 1 C23 C 0.3710(13) 0.604(2) 0.2956(7) 0.015(6) Uiso 0.9513(19) 1 d P A 1 H23A H 0.3772 0.6073 0.2661 0.023 Uiso 0.9513(19) 1 calc PR A 1 H23B H 0.3822 0.6756 0.3078 0.023 Uiso 0.9513(19) 1 calc PR A 1 H23C H 0.3257 0.5861 0.3015 0.023 Uiso 0.9513(19) 1 calc PR A 1 C24 C 0.4029(17) 0.364(3) 0.2857(10) 0.038(8) Uiso 0.9513(19) 1 d P A 1 H24A H 0.4282 0.2999 0.2948 0.057 Uiso 0.9513(19) 1 calc PR A 1 H24B H 0.4126 0.3794 0.2571 0.057 Uiso 0.9513(19) 1 calc PR A 1 H24C H 0.3568 0.3481 0.2887 0.057 Uiso 0.9513(19) 1 calc PR A 1 C25 C 0.5098(14) 0.533(2) 0.3017(9) 0.027(7) Uiso 0.9513(19) 1 d P A 1 H25A H 0.5408 0.4782 0.3121 0.04 Uiso 0.9513(19) 1 calc PR A 1 H25B H 0.52 0.6067 0.3129 0.04 Uiso 0.9513(19) 1 calc PR A 1 H25C H 0.5125 0.5357 0.272 0.04 Uiso 0.9513(19) 1 calc PR A 1 C26 C 0.5160(16) 0.270(3) 0.3623(9) 0.032(8) Uiso 0.9513(19) 1 d P A 1 H26A H 0.5231 0.297 0.3346 0.047 Uiso 0.9513(19) 1 calc PR A 1 H26B H 0.482 0.2129 0.3621 0.047 Uiso 0.9513(19) 1 calc PR A 1 H26C H 0.5561 0.2372 0.3728 0.047 Uiso 0.9513(19) 1 calc PR A 1 C27 C 0.5647(16) 0.468(2) 0.4023(10) 0.032(8) Uiso 0.9513(19) 1 d P A 1 H27A H 0.5767 0.5036 0.3767 0.047 Uiso 0.9513(19) 1 calc PR A 1 H27B H 0.5996 0.4178 0.411 0.047 Uiso 0.9513(19) 1 calc PR A 1 H27C H 0.5576 0.5249 0.4231 0.047 Uiso 0.9513(19) 1 calc PR A 1 C28 C 0.4780(13) 0.332(2) 0.4456(7) 0.015(6) Uiso 0.9513(19) 1 d P A 1 H28A H 0.4385 0.2869 0.4457 0.022 Uiso 0.9513(19) 1 calc PR A 1 H28B H 0.4734 0.3938 0.4649 0.022 Uiso 0.9513(19) 1 calc PR A 1 H28C H 0.5149 0.2857 0.4534 0.022 Uiso 0.9513(19) 1 calc PR A 1 Au1B Au 0.18644(6) 1.14542(9) 0.19279(3) 0.0250(3) Uani 0.9513(19) 1 d P A 1 Au2B Au 0.04353(6) 1.20399(10) 0.17608(3) 0.0297(3) Uani 0.9513(19) 1 d P A 1 Si1B Si 0.0909(4) 0.9300(7) 0.2050(2) 0.0229(19) Uani 0.9513(19) 1 d P A 1 Si2B Si 0.1822(5) 1.0271(7) 0.2732(2) 0.026(2) Uani 0.9513(19) 1 d P A 1 Si3B Si 0.2394(4) 0.9020(6) 0.1969(2) 0.0218(18) Uani 0.9513(19) 1 d P A 1 Si4B Si 0.1395(4) 1.2924(6) 0.1037(2) 0.0166(17) Uani 0.9513(19) 1 d P A 1 Si5B Si 0.0504(4) 1.4536(7) 0.1548(2) 0.0188(18) Uani 0.9513(19) 1 d P A 1 Si6B Si -0.0100(4) 1.2822(7) 0.0919(2) 0.0212(18) Uani 0.9513(19) 1 d P A 1 N1B N 0.0087(11) 1.1075(19) 0.2247(7) 0.024(6) Uiso 0.9513(19) 1 d P A 1 N2B N 0.2200(10) 1.3012(16) 0.1728(6) 0.015(5) Uiso 0.9513(19) 1 d P A 1 C1B C 0.1724(13) 0.989(2) 0.2180(7) 0.009(6) Uiso 0.9513(19) 1 d P A 1 C2B C 0.0633(15) 0.941(3) 0.1508(9) 0.028(7) Uiso 0.9513(19) 1 d P A 1 H2B1 H 0.0203 0.9077 0.1482 0.043 Uiso 0.9513(19) 1 calc PR A 1 H2B2 H 0.0937 0.9008 0.1332 0.043 Uiso 0.9513(19) 1 calc PR A 1 H2B3 H 0.0616 1.0194 0.1428 0.043 Uiso 0.9513(19) 1 calc PR A 1 C3B C 0.0813(17) 0.778(3) 0.2216(10) 0.041(9) Uiso 0.9513(19) 1 d P A 1 H3B1 H 0.038 0.7519 0.2144 0.061 Uiso 0.9513(19) 1 calc PR A 1 H3B2 H 0.0873 0.773 0.251 0.061 Uiso 0.9513(19) 1 calc PR A 1 H3B3 H 0.1138 0.7322 0.2079 0.061 Uiso 0.9513(19) 1 calc PR A 1 C4B C 0.0231(14) 1.005(2) 0.2340(8) 0.011(6) Uiso 0.9513(19) 1 d P A 1 C5B C -0.0069(16) 0.951(3) 0.2685(9) 0.037(8) Uiso 0.9513(19) 1 d P A 1 H5B H 0.0045 0.8775 0.2761 0.045 Uiso 0.9513(19) 1 calc PR A 1 C6B C -0.0500(14) 1.007(2) 0.2887(8) 0.018(6) Uiso 0.9513(19) 1 d P A 1 H6B H -0.0707 0.9697 0.3106 0.021 Uiso 0.9513(19) 1 calc PR A 1 C7B C -0.0681(16) 1.114(3) 0.2815(9) 0.031(7) Uiso 0.9513(19) 1 d P A 1 H7B H -0.0984 1.1526 0.298 0.038 Uiso 0.9513(19) 1 calc PR A 1 C8B C -0.0381(16) 1.163(3) 0.2470(9) 0.032(7) Uiso 0.9513(19) 1 d P A 1 H8B H -0.0504 1.2363 0.2391 0.039 Uiso 0.9513(19) 1 calc PR A 1 C9B C 0.1379(17) 1.151(3) 0.2922(10) 0.042(9) Uiso 0.9513(19) 1 d P A 1 H9B1 H 0.0915 1.1418 0.2871 0.063 Uiso 0.9513(19) 1 calc PR A 1 H9B2 H 0.1533 1.2181 0.2781 0.063 Uiso 0.9513(19) 1 calc PR A 1 H9B3 H 0.1454 1.1595 0.3214 0.063 Uiso 0.9513(19) 1 calc PR A 1 C10B C 0.1620(14) 0.907(2) 0.3083(8) 0.025(7) Uiso 0.9513(19) 1 d P A 1 H10D H 0.1853 0.8399 0.2995 0.037 Uiso 0.9513(19) 1 calc PR A 1 H10E H 0.1154 0.8927 0.3076 0.037 Uiso 0.9513(19) 1 calc PR A 1 H10F H 0.1749 0.9259 0.3361 0.037 Uiso 0.9513(19) 1 calc PR A 1 C11B C 0.2674(15) 1.063(3) 0.2855(9) 0.032(7) Uiso 0.9513(19) 1 d P A 1 H11D H 0.2958 1.0018 0.2766 0.047 Uiso 0.9513(19) 1 calc PR A 1 H11E H 0.2718 1.0731 0.3149 0.047 Uiso 0.9513(19) 1 calc PR A 1 H11F H 0.2795 1.1315 0.2714 0.047 Uiso 0.9513(19) 1 calc PR A 1 C12B C 0.2637(19) 0.776(3) 0.2312(10) 0.046(9) Uiso 0.9513(19) 1 d P A 1 H12D H 0.2992 0.7348 0.2184 0.069 Uiso 0.9513(19) 1 calc PR A 1 H12E H 0.2265 0.7262 0.2346 0.069 Uiso 0.9513(19) 1 calc PR A 1 H12F H 0.2776 0.8033 0.2578 0.069 Uiso 0.9513(19) 1 calc PR A 1 C13B C 0.221(2) 0.835(4) 0.1444(12) 0.060(11) Uiso 0.9513(19) 1 d P A 1 H13D H 0.2584 0.791 0.1356 0.09 Uiso 0.9513(19) 1 calc PR A 1 H13E H 0.2123 0.8938 0.1245 0.09 Uiso 0.9513(19) 1 calc PR A 1 H13F H 0.1832 0.7862 0.1467 0.09 Uiso 0.9513(19) 1 calc PR A 1 C14B C 0.3158(18) 0.984(3) 0.1885(11) 0.045(9) Uiso 0.9513(19) 1 d P A 1 H14D H 0.3494 0.935 0.1777 0.067 Uiso 0.9513(19) 1 calc PR A 1 H14E H 0.3303 1.0164 0.2143 0.067 Uiso 0.9513(19) 1 calc PR A 1 H14F H 0.3075 1.0445 0.169 0.067 Uiso 0.9513(19) 1 calc PR A 1 C15B C 0.0597(13) 1.313(2) 0.1285(7) 0.012(6) Uiso 0.9513(19) 1 d P A 1 C16B C 0.1487(14) 1.367(2) 0.0550(8) 0.019(6) Uiso 0.9513(19) 1 d P A 1 H16D H 0.1917 1.3517 0.0438 0.029 Uiso 0.9513(19) 1 calc PR A 1 H16E H 0.1435 1.4469 0.0595 0.029 Uiso 0.9513(19) 1 calc PR A 1 H16F H 0.1157 1.3405 0.0359 0.029 Uiso 0.9513(19) 1 calc PR A 1 C17B C 0.1711(14) 1.145(2) 0.0953(8) 0.020(6) Uiso 0.9513(19) 1 d P A 1 H17D H 0.2136 1.1479 0.0822 0.03 Uiso 0.9513(19) 1 calc PR A 1 H17E H 0.141 1.1033 0.078 0.03 Uiso 0.9513(19) 1 calc PR A 1 H17F H 0.1751 1.1065 0.1216 0.03 Uiso 0.9513(19) 1 calc PR A 1 C18B C 0.2057(13) 1.347(2) 0.1385(8) 0.015(6) Uiso 0.9513(19) 1 d P A 1 C19B C 0.2366(16) 1.448(3) 0.1295(9) 0.033(8) Uiso 0.9513(19) 1 d P A 1 H19B H 0.2289 1.4829 0.1041 0.039 Uiso 0.9513(19) 1 calc PR A 1 C20B C 0.2823(18) 1.501(3) 0.1597(10) 0.034(8) Uiso 0.9513(19) 1 d P A 1 H20B H 0.3032 1.5698 0.1543 0.041 Uiso 0.9513(19) 1 calc PR A 1 C21B C 0.2907(19) 1.450(3) 0.1920(12) 0.055(10) Uiso 0.9513(19) 1 d P A 1 H21B H 0.3181 1.4804 0.2122 0.066 Uiso 0.9513(19) 1 calc PR A 1 C22B C 0.2596(14) 1.343(2) 0.1993(9) 0.030(7) Uiso 0.9513(19) 1 d P A 1 H22B H 0.2682 1.3037 0.2238 0.036 Uiso 0.9513(19) 1 calc PR A 1 C23B C 0.0081(15) 1.161(2) 0.0559(9) 0.029(7) Uiso 0.9513(19) 1 d P A 1 H23D H 0.047 1.1783 0.0402 0.044 Uiso 0.9513(19) 1 calc PR A 1 H23E H -0.0285 1.1509 0.0373 0.044 Uiso 0.9513(19) 1 calc PR A 1 H23F H 0.0149 1.0931 0.0716 0.044 Uiso 0.9513(19) 1 calc PR A 1 C24B C -0.0859(18) 1.240(3) 0.1193(11) 0.048(9) Uiso 0.9513(19) 1 d P A 1 H24D H -0.077 1.1742 0.1363 0.072 Uiso 0.9513(19) 1 calc PR A 1 H24E H -0.1195 1.221 0.0995 0.072 Uiso 0.9513(19) 1 calc PR A 1 H24F H -0.1008 1.3012 0.1365 0.072 Uiso 0.9513(19) 1 calc PR A 1 C25B C -0.0296(14) 1.408(2) 0.0593(8) 0.022(6) Uiso 0.9513(19) 1 d P A 1 H25D H 0.0092 1.431 0.0445 0.033 Uiso 0.9513(19) 1 calc PR A 1 H25E H -0.0445 1.469 0.0766 0.033 Uiso 0.9513(19) 1 calc PR A 1 H25F H -0.0636 1.3881 0.0399 0.033 Uiso 0.9513(19) 1 calc PR A 1 C26B C -0.0337(13) 1.477(2) 0.1712(8) 0.019(6) Uiso 0.9513(19) 1 d P A 1 H26D H -0.037 1.5495 0.1846 0.029 Uiso 0.9513(19) 1 calc PR A 1 H26E H -0.0465 1.4179 0.1901 0.029 Uiso 0.9513(19) 1 calc PR A 1 H26F H -0.0622 1.4754 0.1474 0.029 Uiso 0.9513(19) 1 calc PR A 1 C27B C 0.1016(13) 1.472(2) 0.2032(7) 0.013(6) Uiso 0.9513(19) 1 d P A 1 H27D H 0.1474 1.462 0.1965 0.02 Uiso 0.9513(19) 1 calc PR A 1 H27E H 0.0887 1.4161 0.2234 0.02 Uiso 0.9513(19) 1 calc PR A 1 H27F H 0.0948 1.5468 0.2143 0.02 Uiso 0.9513(19) 1 calc PR A 1 C28B C 0.0734(14) 1.577(2) 0.1213(8) 0.024(7) Uiso 0.9513(19) 1 d P A 1 H28D H 0.1181 1.5685 0.112 0.036 Uiso 0.9513(19) 1 calc PR A 1 H28E H 0.0694 1.6464 0.1369 0.036 Uiso 0.9513(19) 1 calc PR A 1 H28F H 0.0445 1.5801 0.0977 0.036 Uiso 0.9513(19) 1 calc PR A 1 Au1C Au 0.2896(10) 0.3233(16) 0.4176(11) 0.018(5) Uiso 0.0487(19) 1 d P A 2 Au2C Au 0.4311(11) 0.3767(17) 0.3960(12) 0.023(6) Uiso 0.0487(19) 1 d P A 2 Au1D Au 0.1879(9) 0.8632(14) 0.1951(9) 0.006(5) Uiso 0.0487(19) 1 d P A 2 Au2D Au 0.0455(10) 0.7984(15) 0.1762(9) 0.012(5) Uiso 0.0487(19) 1 d P A 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0272(7) 0.0263(6) 0.0200(6) -0.0008(5) 0.0002(5) 0.0025(5) Au2 0.0240(6) 0.0232(6) 0.0181(6) 0.0002(5) 0.0034(5) 0.0033(5) Si1 0.022(4) 0.013(4) 0.008(4) -0.002(3) 0.000(3) 0.001(3) Si2 0.027(5) 0.025(4) 0.010(4) 0.005(3) 0.002(3) -0.002(4) Si3 0.023(5) 0.023(4) 0.011(4) 0.002(3) -0.002(3) 0.007(4) Si4 0.032(5) 0.010(4) 0.014(4) -0.004(3) -0.001(3) -0.003(3) Si5 0.022(5) 0.030(4) 0.003(4) 0.009(3) 0.000(3) 0.000(4) Si6 0.032(5) 0.070(7) 0.022(4) -0.011(5) -0.013(4) 0.027(5) Au1B 0.0278(7) 0.0274(6) 0.0198(6) 0.0010(5) 0.0000(5) -0.0004(5) Au2B 0.0330(7) 0.0306(7) 0.0255(6) 0.0023(5) 0.0012(5) -0.0016(6) Si1B 0.026(5) 0.032(5) 0.010(4) 0.002(3) 0.000(3) 0.006(4) Si2B 0.031(6) 0.039(5) 0.009(4) -0.003(3) -0.005(4) -0.003(4) Si3B 0.043(6) 0.004(3) 0.019(4) -0.001(3) 0.005(4) 0.004(4) Si4B 0.015(4) 0.028(4) 0.007(4) -0.001(3) 0.000(3) 0.001(3) Si5B 0.017(5) 0.029(5) 0.010(4) -0.001(3) 0.004(3) 0.000(4) Si6B 0.024(5) 0.026(4) 0.015(4) 0.003(3) -0.003(3) -0.005(4) #----------------------------------------------------------------------------# # 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 Au1 C1 2.05(2) . ? Au1 N2 2.09(2) . ? Au1 Au2 3.0749(16) . ? Au1 Si3 3.096(8) . ? Au2 C15 2.07(3) . ? Au2 N1 2.14(2) . ? Au2 Si5 3.061(8) . ? Si1 C3 1.87(3) . ? Si1 C1 1.90(3) . ? Si1 C2 1.90(3) . ? Si1 C4 1.93(3) . ? Si2 C1 1.88(3) . ? Si2 C9 1.89(3) . ? Si2 C10 1.93(3) . ? Si2 C11 1.93(3) . ? Si3 C13 1.83(3) . ? Si3 C12 1.87(3) . ? Si3 C14 1.88(3) . ? Si3 C1 1.91(2) . ? Si4 C16 1.84(3) . ? Si4 C17 1.84(3) . ? Si4 C15 1.87(3) . ? Si4 C18 1.89(3) . ? Si5 C15 1.89(3) . ? Si5 C23 1.89(3) . ? Si5 C24 1.90(3) . ? Si5 C25 1.91(3) . ? Si6 C28 1.81(3) . ? Si6 C27 1.82(3) . ? Si6 C26 1.86(3) . ? Si6 C15 1.89(3) . ? N1 C4 1.33(3) . ? N1 C8 1.38(4) . ? N2 C22 1.35(4) . ? N2 C18 1.40(4) . ? C4 C5 1.46(4) . ? C5 C6 1.29(5) . ? C6 C7 1.44(5) . ? C7 C8 1.36(4) . ? C18 C19 1.36(4) . ? C19 C20 1.43(5) . ? C20 C21 1.30(4) . ? C21 C22 1.45(4) . ? Au1B C1B 2.07(2) . ? Au1B N2B 2.10(2) . ? Au1B Si2B 3.005(8) . ? Au1B Au2B 3.0905(18) . ? Au2B C15B 2.07(2) . ? Au2B N1B 2.10(2) . ? Au2B Si5B 3.077(8) . ? Si1B C2B 1.88(3) . ? Si1B C1B 1.88(3) . ? Si1B C3B 1.91(3) . ? Si1B C4B 1.92(3) . ? Si2B C9B 1.86(3) . ? Si2B C11B 1.86(3) . ? Si2B C1B 1.89(3) . ? Si2B C10B 1.90(3) . ? Si3B C1B 1.87(3) . ? Si3B C14B 1.89(4) . ? Si3B C13B 1.94(4) . ? Si3B C12B 1.95(4) . ? Si4B C16B 1.84(3) . ? Si4B C15B 1.86(3) . ? Si4B C18B 1.90(3) . ? Si4B C17B 1.91(3) . ? Si5B C26B 1.84(3) . ? Si5B C15B 1.90(2) . ? Si5B C28B 1.91(3) . ? Si5B C27B 1.93(2) . ? Si6B C24B 1.88(4) . ? Si6B C25B 1.89(3) . ? Si6B C23B 1.91(3) . ? Si6B C15B 1.92(3) . ? N1B C4B 1.31(3) . ? N1B C8B 1.39(4) . ? N2B C18B 1.29(3) . ? N2B C22B 1.30(3) . ? C4B C5B 1.44(4) . ? C5B C6B 1.30(4) . ? C6B C7B 1.36(4) . ? C7B C8B 1.42(4) . ? C18B C19B 1.40(4) . ? C19B C20B 1.51(5) . ? C20B C21B 1.24(5) . ? C21B C22B 1.45(5) . ? Au1C Au2C 3.08(3) . ? Au1D Au2D 3.11(3) . ? 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 C1 Au1 N2 168.5(9) . . ? C1 Au1 Au2 99.9(7) . . ? N2 Au1 Au2 90.7(6) . . ? C1 Au1 Si3 36.9(7) . . ? N2 Au1 Si3 136.1(6) . . ? Au2 Au1 Si3 104.04(16) . . ? C15 Au2 N1 167.7(10) . . ? C15 Au2 Si5 37.2(8) . . ? N1 Au2 Si5 136.0(6) . . ? C15 Au2 Au1 100.3(8) . . ? N1 Au2 Au1 91.5(6) . . ? Si5 Au2 Au1 105.87(18) . . ? C3 Si1 C1 115.9(12) . . ? C3 Si1 C2 104.2(13) . . ? C1 Si1 C2 115.3(12) . . ? C3 Si1 C4 105.4(12) . . ? C1 Si1 C4 108.7(12) . . ? C2 Si1 C4 106.6(13) . . ? C1 Si2 C9 111.6(13) . . ? C1 Si2 C10 113.5(13) . . ? C9 Si2 C10 105.8(13) . . ? C1 Si2 C11 112.1(11) . . ? C9 Si2 C11 106.7(13) . . ? C10 Si2 C11 106.5(13) . . ? C13 Si3 C12 105.5(14) . . ? C13 Si3 C14 107.0(13) . . ? C12 Si3 C14 105.7(14) . . ? C13 Si3 C1 112.3(12) . . ? C12 Si3 C1 110.2(13) . . ? C14 Si3 C1 115.6(12) . . ? C13 Si3 Au1 83.2(9) . . ? C12 Si3 Au1 93.7(10) . . ? C14 Si3 Au1 154.3(10) . . ? C1 Si3 Au1 40.0(7) . . ? C16 Si4 C17 106.2(13) . . ? C16 Si4 C15 117.1(14) . . ? C17 Si4 C15 112.0(12) . . ? C16 Si4 C18 107.5(14) . . ? C17 Si4 C18 105.1(12) . . ? C15 Si4 C18 108.2(13) . . ? C15 Si5 C23 117.1(12) . . ? C15 Si5 C24 114.2(13) . . ? C23 Si5 C24 102.7(13) . . ? C15 Si5 C25 111.0(13) . . ? C23 Si5 C25 104.5(12) . . ? C24 Si5 C25 106.3(14) . . ? C15 Si5 Au2 41.4(8) . . ? C23 Si5 Au2 88.4(8) . . ? C24 Si5 Au2 154.7(11) . . ? C25 Si5 Au2 92.5(9) . . ? C28 Si6 C27 101.7(14) . . ? C28 Si6 C26 107.4(14) . . ? C27 Si6 C26 104.1(15) . . ? C28 Si6 C15 114.1(13) . . ? C27 Si6 C15 115.9(14) . . ? C26 Si6 C15 112.5(14) . . ? C4 N1 C8 119(2) . . ? C4 N1 Au2 126.4(18) . . ? C8 N1 Au2 113.6(18) . . ? C22 N2 C18 118(2) . . ? C22 N2 Au1 113.2(19) . . ? C18 N2 Au1 129.0(18) . . ? Si2 C1 Si1 112.7(13) . . ? Si2 C1 Si3 111.2(13) . . ? Si1 C1 Si3 111.5(13) . . ? Si2 C1 Au1 105.8(12) . . ? Si1 C1 Au1 111.9(12) . . ? Si3 C1 Au1 103.1(11) . . ? N1 C4 C5 121(3) . . ? N1 C4 Si1 121(2) . . ? C5 C4 Si1 118(2) . . ? C6 C5 C4 119(3) . . ? C5 C6 C7 120(3) . . ? C8 C7 C6 120(3) . . ? C7 C8 N1 120(3) . . ? Si4 C15 Si5 112.4(15) . . ? Si4 C15 Si6 112.6(14) . . ? Si5 C15 Si6 113.7(15) . . ? Si4 C15 Au2 111.8(14) . . ? Si5 C15 Au2 101.4(12) . . ? Si6 C15 Au2 104.0(13) . . ? C19 C18 N2 118(3) . . ? C19 C18 Si4 123(2) . . ? N2 C18 Si4 119(2) . . ? C18 C19 C20 125(3) . . ? C21 C20 C19 116(3) . . ? C20 C21 C22 121(3) . . ? N2 C22 C21 122(3) . . ? C1B Au1B N2B 168.0(9) . . ? C1B Au1B Si2B 38.4(7) . . ? N2B Au1B Si2B 134.9(6) . . ? C1B Au1B Au2B 98.2(7) . . ? N2B Au1B Au2B 93.4(6) . . ? Si2B Au1B Au2B 103.66(19) . . ? C15B Au2B N1B 168.6(10) . . ? C15B Au2B Si5B 37.3(7) . . ? N1B Au2B Si5B 136.4(6) . . ? C15B Au2B Au1B 97.1(7) . . ? N1B Au2B Au1B 93.9(6) . . ? Si5B Au2B Au1B 102.57(16) . . ? C2B Si1B C1B 117.7(13) . . ? C2B Si1B C3B 107.8(14) . . ? C1B Si1B C3B 112.7(14) . . ? C2B Si1B C4B 102.6(13) . . ? C1B Si1B C4B 111.6(12) . . ? C3B Si1B C4B 103.0(13) . . ? C9B Si2B C11B 102.2(15) . . ? C9B Si2B C1B 117.8(14) . . ? C11B Si2B C1B 111.5(13) . . ? C9B Si2B C10B 107.1(14) . . ? C11B Si2B C10B 104.5(14) . . ? C1B Si2B C10B 112.4(12) . . ? C9B Si2B Au1B 86.2(11) . . ? C11B Si2B Au1B 93.2(10) . . ? C1B Si2B Au1B 42.9(7) . . ? C10B Si2B Au1B 154.6(9) . . ? C1B Si3B C14B 112.7(13) . . ? C1B Si3B C13B 114.6(16) . . ? C14B Si3B C13B 104.4(17) . . ? C1B Si3B C12B 114.1(14) . . ? C14B Si3B C12B 105.9(16) . . ? C13B Si3B C12B 104.1(17) . . ? C16B Si4B C15B 114.1(12) . . ? C16B Si4B C18B 106.5(12) . . ? C15B Si4B C18B 109.2(11) . . ? C16B Si4B C17B 106.7(12) . . ? C15B Si4B C17B 119.5(12) . . ? C18B Si4B C17B 99.1(12) . . ? C26B Si5B C15B 111.3(12) . . ? C26B Si5B C28B 106.7(13) . . ? C15B Si5B C28B 113.5(12) . . ? C26B Si5B C27B 105.1(12) . . ? C15B Si5B C27B 114.9(11) . . ? C28B Si5B C27B 104.6(12) . . ? C26B Si5B Au2B 92.1(9) . . ? C15B Si5B Au2B 41.2(7) . . ? C28B Si5B Au2B 154.0(9) . . ? C27B Si5B Au2B 87.0(8) . . ? C24B Si6B C25B 108.1(15) . . ? C24B Si6B C23B 104.9(15) . . ? C25B Si6B C23B 107.0(13) . . ? C24B Si6B C15B 112.3(14) . . ? C25B Si6B C15B 111.3(12) . . ? C23B Si6B C15B 113.0(13) . . ? C4B N1B C8B 119(2) . . ? C4B N1B Au2B 128.3(19) . . ? C8B N1B Au2B 112.3(19) . . ? C18B N2B C22B 125(2) . . ? C18B N2B Au1B 125.2(17) . . ? C22B N2B Au1B 110.0(18) . . ? Si3B C1B Si1B 111.8(13) . . ? Si3B C1B Si2B 114.4(14) . . ? Si1B C1B Si2B 114.0(14) . . ? Si3B C1B Au1B 104.6(12) . . ? Si1B C1B Au1B 112.1(13) . . ? Si2B C1B Au1B 98.7(11) . . ? N1B C4B C5B 120(3) . . ? N1B C4B Si1B 119(2) . . ? C5B C4B Si1B 120(2) . . ? C6B C5B C4B 118(3) . . ? C5B C6B C7B 126(3) . . ? C6B C7B C8B 114(3) . . ? N1B C8B C7B 122(3) . . ? Si4B C15B Si5B 114.1(13) . . ? Si4B C15B Si6B 111.5(12) . . ? Si5B C15B Si6B 112.4(13) . . ? Si4B C15B Au2B 113.1(12) . . ? Si5B C15B Au2B 101.5(11) . . ? Si6B C15B Au2B 103.4(12) . . ? N2B C18B C19B 117(2) . . ? N2B C18B Si4B 123.2(19) . . ? C19B C18B Si4B 120(2) . . ? C18B C19B C20B 121(3) . . ? C21B C20B C19B 116(3) . . ? C20B C21B C22B 121(4) . . ? N2B C22B C21B 121(3) . . ? #===END data_ce-jds-4 _database_code_CSD 177598 _audit_creation_date 2000-06-09T08:40:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{ZnBr(C(SiMe3)2(SiMe2C5H4N))}2]' _chemical_formula_moiety 'C28 H56 Br2 N2 Si6 Zn2' _chemical_formula_structural 'C28 H56 BR2 N2 SI6 ZN2' _chemical_formula_sum 'C28 H56 Br2 N2 Si6 Zn2' _chemical_formula_weight 879.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2402(9) _cell_length_b 9.5269(8) _cell_length_c 12.2376(11) _cell_angle_alpha 79.992(6) _cell_angle_beta 77.626(5) _cell_angle_gamma 87.953(6) _cell_volume 1036.24(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10931 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.365 _exptl_absorpt_correction_T_max 0.443 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 7343 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0602 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.942 _diffrn_measured_fraction_theta_max 0.942 _reflns_number_total 4655 _reflns_number_gt 3806 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0612P)^2^+1.4208P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4655 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.136 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.853 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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' 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 Zn Zn 0.11259(5) 0.13028(5) -0.09395(4) 0.03578(15) Uani 1 1 d . . . Br Br 0.13956(5) -0.13406(5) -0.02262(4) 0.04954(17) Uani 1 1 d . . . Si1 Si 0.39429(12) 0.24964(15) -0.23384(11) 0.0457(3) Uani 1 1 d . . . Si2 Si 0.1786(2) 0.12867(17) -0.36375(12) 0.0591(4) Uani 1 1 d . . . Si3 Si 0.10813(13) 0.41131(13) -0.26469(11) 0.0397(3) Uani 1 1 d . . . N N 0.2517(4) 0.2081(4) -0.0057(3) 0.0398(8) Uani 1 1 d . . . C1 C 0.2026(4) 0.2328(4) -0.2533(3) 0.0348(8) Uani 1 1 d . . . C2 C 0.5021(6) 0.4122(8) -0.3175(6) 0.085(2) Uani 1 1 d . . . H2A H 0.6014 0.4094 -0.3008 0.128 Uiso 1 1 calc R . . H2B H 0.4505 0.4983 -0.2963 0.128 Uiso 1 1 calc R . . H2C H 0.5105 0.4131 -0.3988 0.128 Uiso 1 1 calc R . . C3 C 0.5183(8) 0.0929(9) -0.2534(7) 0.096(3) Uani 1 1 d . . . H3A H 0.6161 0.1135 -0.241 0.145 Uiso 1 1 calc R . . H3B H 0.5282 0.0736 -0.3308 0.145 Uiso 1 1 calc R . . H3C H 0.4757 0.0093 -0.1988 0.145 Uiso 1 1 calc R . . C4 C 0.3792(5) 0.2585(5) -0.0777(4) 0.0437(10) Uani 1 1 d . . . C5 C 0.4901(6) 0.3084(6) -0.0312(6) 0.0631(15) Uani 1 1 d . . . H5 H 0.5806 0.3437 -0.0797 0.076 Uiso 1 1 calc R . . C6 C 0.4695(8) 0.3067(7) 0.0823(6) 0.0737(18) Uani 1 1 d . . . H6 H 0.5454 0.34 0.1129 0.088 Uiso 1 1 calc R . . C7 C 0.3389(8) 0.2569(7) 0.1526(5) 0.0682(17) Uani 1 1 d . . . H7 H 0.3222 0.2568 0.2319 0.082 Uiso 1 1 calc R . . C8 C 0.2317(6) 0.2068(6) 0.1054(4) 0.0536(12) Uani 1 1 d . . . H8 H 0.1414 0.1706 0.1537 0.064 Uiso 1 1 calc R . . C9 C -0.0248(11) 0.1215(12) -0.3730(9) 0.131(4) Uani 1 1 d . . . H9A H -0.0845 0.0833 -0.298 0.196 Uiso 1 1 calc R . . H9B H -0.0352 0.0598 -0.4271 0.196 Uiso 1 1 calc R . . H9C H -0.0589 0.2178 -0.3986 0.196 Uiso 1 1 calc R . . C10 C 0.2830(13) 0.2029(9) -0.5084(6) 0.128(4) Uani 1 1 d . . . H10A H 0.2588 0.304 -0.5268 0.193 Uiso 1 1 calc R . . H10B H 0.2557 0.1512 -0.5636 0.193 Uiso 1 1 calc R . . H10C H 0.3896 0.1926 -0.5111 0.193 Uiso 1 1 calc R . . C11 C 0.2366(12) -0.0611(7) -0.3414(7) 0.108(3) Uani 1 1 d . . . H11A H 0.1854 -0.1086 -0.2661 0.162 Uiso 1 1 calc R . . H11B H 0.3439 -0.0663 -0.3465 0.162 Uiso 1 1 calc R . . H11C H 0.211 -0.1084 -0.3997 0.162 Uiso 1 1 calc R . . C12 C -0.0994(6) 0.4035(7) -0.2408(7) 0.088(2) Uani 1 1 d . . . H12A H -0.1389 0.3437 -0.1674 0.132 Uiso 1 1 calc R . . H12B H -0.1273 0.3626 -0.3016 0.132 Uiso 1 1 calc R . . H12C H -0.14 0.4999 -0.241 0.132 Uiso 1 1 calc R . . C13 C 0.1663(7) 0.5286(6) -0.4060(5) 0.0673(16) Uani 1 1 d . . . H13A H 0.2743 0.5391 -0.4244 0.101 Uiso 1 1 calc R . . H13B H 0.1201 0.6225 -0.4031 0.101 Uiso 1 1 calc R . . H13C H 0.1348 0.4857 -0.4643 0.101 Uiso 1 1 calc R . . C14 C 0.1415(8) 0.5143(6) -0.1553(5) 0.0701(16) Uani 1 1 d . . . H14A H 0.2483 0.5227 -0.1609 0.105 Uiso 1 1 calc R . . H14B H 0.0953 0.4644 -0.0795 0.105 Uiso 1 1 calc R . . H14C H 0.0982 0.6096 -0.1682 0.105 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 Zn 0.0292(2) 0.0375(3) 0.0363(3) 0.00245(19) -0.00314(18) -0.00810(18) Br 0.0341(2) 0.0379(2) 0.0628(3) 0.0061(2) 0.00790(19) 0.00265(17) Si1 0.0249(5) 0.0546(8) 0.0480(7) 0.0070(6) 0.0011(5) -0.0003(5) Si2 0.0858(11) 0.0520(8) 0.0389(7) -0.0080(6) -0.0103(7) -0.0080(7) Si3 0.0330(6) 0.0385(6) 0.0435(7) 0.0049(5) -0.0085(5) -0.0008(4) N 0.0383(18) 0.0402(19) 0.0405(19) 0.0004(15) -0.0124(15) -0.0059(15) C1 0.0287(18) 0.039(2) 0.035(2) -0.0008(17) -0.0058(15) -0.0059(15) C2 0.039(3) 0.110(5) 0.083(4) 0.039(4) -0.001(3) -0.030(3) C3 0.066(4) 0.111(6) 0.103(6) -0.016(5) -0.006(4) 0.045(4) C4 0.031(2) 0.040(2) 0.058(3) 0.004(2) -0.0150(19) -0.0007(16) C5 0.046(3) 0.066(3) 0.083(4) 0.000(3) -0.033(3) -0.009(2) C6 0.074(4) 0.076(4) 0.087(5) -0.012(3) -0.052(4) -0.009(3) C7 0.095(5) 0.065(4) 0.055(3) -0.012(3) -0.040(3) 0.017(3) C8 0.062(3) 0.055(3) 0.044(3) -0.003(2) -0.016(2) 0.002(2) C9 0.129(8) 0.165(10) 0.136(8) -0.081(8) -0.062(7) -0.026(7) C10 0.232(12) 0.089(6) 0.041(4) -0.014(4) 0.027(5) -0.020(7) C11 0.199(10) 0.052(4) 0.082(5) -0.025(4) -0.039(6) 0.012(5) C12 0.040(3) 0.078(4) 0.127(6) 0.035(4) -0.018(3) 0.007(3) C13 0.078(4) 0.057(3) 0.057(3) 0.017(3) -0.016(3) -0.002(3) C14 0.097(5) 0.054(3) 0.063(4) -0.015(3) -0.024(3) 0.020(3) #----------------------------------------------------------------------------# # 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 Zn C1 2.037(4) . ? Zn N 2.077(4) . ? Zn Br 2.4601(6) 2 ? Zn Br 2.5398(7) . ? Zn Si1 2.9367(12) . ? Br Zn 2.4601(6) 2 ? Si1 C1 1.853(4) . ? Si1 C3 1.867(7) . ? Si1 C2 1.887(6) . ? Si1 C4 1.902(5) . ? Si2 C10 1.856(7) . ? Si2 C11 1.858(7) . ? Si2 C1 1.862(5) . ? Si2 C9 1.911(9) . ? Si3 C13 1.871(5) . ? Si3 C14 1.872(6) . ? Si3 C12 1.879(6) . ? Si3 C1 1.881(4) . ? N C8 1.330(6) . ? N C4 1.358(6) . ? C4 C5 1.407(7) . ? C5 C6 1.358(9) . ? C6 C7 1.369(10) . ? C7 C8 1.384(8) . ? 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 C1 Zn N 98.97(15) . . ? C1 Zn Br 131.30(11) . 2 ? N Zn Br 106.42(11) . 2 ? C1 Zn Br 124.99(12) . . ? N Zn Br 98.45(10) . . ? Br Zn Br 91.79(2) 2 . ? C1 Zn Si1 38.68(11) . . ? N Zn Si1 64.92(11) . . ? Br Zn Si1 156.70(4) 2 . ? Br Zn Si1 110.53(3) . . ? Zn Br Zn 88.21(2) 2 . ? C1 Si1 C3 116.5(3) . . ? C1 Si1 C2 116.7(2) . . ? C3 Si1 C2 106.8(4) . . ? C1 Si1 C4 106.50(19) . . ? C3 Si1 C4 102.3(3) . . ? C2 Si1 C4 106.7(3) . . ? C1 Si1 Zn 43.40(12) . . ? C3 Si1 Zn 105.3(3) . . ? C2 Si1 Zn 147.9(2) . . ? C4 Si1 Zn 68.29(13) . . ? C10 Si2 C11 104.3(4) . . ? C10 Si2 C1 113.6(3) . . ? C11 Si2 C1 115.8(3) . . ? C10 Si2 C9 106.6(5) . . ? C11 Si2 C9 104.4(5) . . ? C1 Si2 C9 111.2(3) . . ? C13 Si3 C14 106.9(3) . . ? C13 Si3 C12 104.4(3) . . ? C14 Si3 C12 103.8(4) . . ? C13 Si3 C1 114.1(3) . . ? C14 Si3 C1 111.9(2) . . ? C12 Si3 C1 114.8(2) . . ? C8 N C4 121.1(4) . . ? C8 N Zn 128.5(3) . . ? C4 N Zn 110.3(3) . . ? Si1 C1 Si2 116.5(2) . . ? Si1 C1 Si3 110.7(2) . . ? Si2 C1 Si3 113.6(2) . . ? Si1 C1 Zn 97.92(18) . . ? Si2 C1 Zn 111.7(2) . . ? Si3 C1 Zn 104.6(2) . . ? N C4 C5 117.9(5) . . ? N C4 Si1 116.5(3) . . ? C5 C4 Si1 125.5(4) . . ? C6 C5 C4 120.8(6) . . ? C5 C6 C7 119.8(5) . . ? C6 C7 C8 118.6(6) . . ? N C8 C7 121.7(5) . . ? #===END data_ce-jds-5 _database_code_CSD 177599 _audit_creation_date 2000-04-11T14:36:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{CdCl(C(SiMe3)2(SiMe2C5H4N))}2]' _chemical_formula_moiety 'C28 H56 Cd2 Cl2 N2 Si6' _chemical_formula_structural 'C28 H56 CD2 CL2 N2 SI6' _chemical_formula_sum 'C28 H56 Cd2 Cl2 N2 Si6' _chemical_formula_weight 884.99 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.4324(4) _cell_length_b 8.8552(3) _cell_length_c 18.0063(5) _cell_angle_alpha 90 _cell_angle_beta 100.072(2) _cell_angle_gamma 90 _cell_volume 2108.78(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26430 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.810 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 25201 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 3711 _reflns_number_gt 3155 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0788P)^2^+9.8902P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3711 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.058 _refine_ls_wR_factor_ref 0.161 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.259 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.13 #----------------------------------------------------------------------------# # 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' Cd Cd -0.8075 1.2024 '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' 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' 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 Cd Cd 0.12001(3) 0.06649(6) 0.05550(2) 0.0428(2) Uani 1 1 d . . . Cl Cl -0.07023(10) 0.1273(2) 0.05009(8) 0.0528(5) Uani 1 1 d . . . Si1 Si 0.33297(13) 0.0645(2) 0.15493(10) 0.0442(4) Uani 1 1 d . . . Si2 Si 0.3190(2) 0.2495(3) 0.00725(15) 0.0763(7) Uani 1 1 d . . . Si3 Si 0.21390(16) 0.3668(2) 0.13975(13) 0.0575(5) Uani 1 1 d . . . N N 0.1493(5) -0.0730(6) 0.1657(3) 0.0521(14) Uani 1 1 d . . . C1 C 0.2588(5) 0.2012(7) 0.0904(4) 0.0435(14) Uani 1 1 d . . . C2 C 0.4296(6) 0.1477(12) 0.2322(6) 0.087(3) Uani 1 1 d . . . H2A H 0.4645 0.0663 0.2632 0.131 Uiso 1 1 calc R . . H2B H 0.3958 0.2139 0.2637 0.131 Uiso 1 1 calc R . . H2C H 0.4788 0.2064 0.21 0.131 Uiso 1 1 calc R . . C3 C 0.3973(6) -0.0856(9) 0.1078(5) 0.065(2) Uani 1 1 d . . . H3A H 0.4342 -0.1533 0.1461 0.098 Uiso 1 1 calc R . . H3B H 0.4448 -0.0387 0.0792 0.098 Uiso 1 1 calc R . . H3C H 0.3466 -0.1435 0.0735 0.098 Uiso 1 1 calc R . . C4 C 0.2445(5) -0.0510(7) 0.2046(4) 0.0460(15) Uani 1 1 d . . . C5 C 0.2726(7) -0.1183(9) 0.2744(4) 0.064(2) Uani 1 1 d . . . H5 H 0.3386 -0.1017 0.3021 0.077 Uiso 1 1 calc R . . C6 C 0.2070(10) -0.2081(11) 0.3043(5) 0.084(3) Uani 1 1 d . . . H6 H 0.2273 -0.2546 0.3521 0.101 Uiso 1 1 calc R . . C7 C 0.1133(10) -0.2300(11) 0.2652(5) 0.089(3) Uani 1 1 d . . . H7 H 0.0664 -0.2918 0.285 0.106 Uiso 1 1 calc R . . C8 C 0.0860(7) -0.1610(10) 0.1955(5) 0.072(2) Uani 1 1 d . . . H8 H 0.0198 -0.1771 0.1679 0.086 Uiso 1 1 calc R . . C9 C 0.3124(8) 0.0927(12) -0.0633(5) 0.085(3) Uani 1 1 d . . . H9A H 0.3445 0.1252 -0.1055 0.128 Uiso 1 1 calc R . . H9B H 0.2415 0.0672 -0.0821 0.128 Uiso 1 1 calc R . . H9C H 0.3477 0.0039 -0.0392 0.128 Uiso 1 1 calc R . . C10 C 0.4567(9) 0.2999(14) 0.0387(8) 0.116(4) Uani 1 1 d . . . H10A H 0.4869 0.3251 -0.0055 0.174 Uiso 1 1 calc R . . H10B H 0.4925 0.2138 0.0652 0.174 Uiso 1 1 calc R . . H10C H 0.462 0.3871 0.0727 0.174 Uiso 1 1 calc R . . C11 C 0.2555(15) 0.4143(15) -0.0481(9) 0.166(8) Uani 1 1 d . . . H11A H 0.2891 0.4348 -0.0911 0.25 Uiso 1 1 calc R . . H11B H 0.2602 0.5037 -0.0155 0.25 Uiso 1 1 calc R . . H11C H 0.1842 0.3902 -0.0663 0.25 Uiso 1 1 calc R . . C12 C 0.3151(9) 0.5119(12) 0.1661(8) 0.111(4) Uani 1 1 d . . . H12A H 0.2882 0.5968 0.1913 0.166 Uiso 1 1 calc R . . H12B H 0.3381 0.5481 0.1204 0.166 Uiso 1 1 calc R . . H12C H 0.3722 0.4669 0.2002 0.166 Uiso 1 1 calc R . . C13 C 0.0994(8) 0.4637(11) 0.0854(6) 0.090(3) Uani 1 1 d . . . H13A H 0.0451 0.3897 0.0714 0.135 Uiso 1 1 calc R . . H13B H 0.1166 0.5092 0.0397 0.135 Uiso 1 1 calc R . . H13C H 0.0768 0.5426 0.1168 0.135 Uiso 1 1 calc R . . C14 C 0.1735(7) 0.3065(11) 0.2297(5) 0.074(2) Uani 1 1 d . . . H14A H 0.1195 0.2312 0.2185 0.111 Uiso 1 1 calc R . . H14B H 0.1486 0.3944 0.254 0.111 Uiso 1 1 calc R . . H14C H 0.2313 0.2624 0.2635 0.111 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 Cd 0.0361(3) 0.0590(3) 0.0303(3) -0.00627(18) -0.00207(18) -0.00646(19) Cl 0.0250(7) 0.0919(12) 0.0418(8) -0.0467(8) 0.0068(5) -0.0005(7) Si1 0.0374(9) 0.0447(10) 0.0460(10) 0.0038(7) -0.0049(7) -0.0029(7) Si2 0.0921(17) 0.0657(14) 0.0790(16) 0.0298(12) 0.0370(13) -0.0073(12) Si3 0.0570(11) 0.0363(10) 0.0736(14) -0.0032(9) -0.0040(10) -0.0038(8) N 0.068(4) 0.045(3) 0.046(3) 0.004(2) 0.016(3) -0.012(3) C1 0.042(3) 0.038(3) 0.049(3) 0.007(3) 0.004(3) -0.007(3) C2 0.051(5) 0.104(7) 0.093(7) -0.012(6) -0.026(4) -0.005(5) C3 0.062(5) 0.055(4) 0.081(6) 0.015(4) 0.018(4) 0.010(3) C4 0.062(4) 0.039(3) 0.035(3) -0.002(3) 0.001(3) 0.001(3) C5 0.100(6) 0.055(4) 0.038(4) 0.006(3) 0.013(4) 0.013(4) C6 0.144(9) 0.066(5) 0.048(4) 0.015(4) 0.033(5) 0.014(6) C7 0.144(10) 0.069(6) 0.067(6) 0.015(5) 0.055(6) -0.013(6) C8 0.085(6) 0.070(5) 0.070(5) -0.007(4) 0.039(4) -0.022(4) C9 0.091(7) 0.120(8) 0.051(5) 0.019(5) 0.032(4) -0.006(6) C10 0.107(8) 0.104(8) 0.155(11) -0.007(8) 0.071(8) -0.052(7) C11 0.27(2) 0.123(11) 0.133(11) 0.094(10) 0.107(12) 0.065(12) C12 0.106(8) 0.059(6) 0.165(12) -0.028(7) 0.014(8) -0.024(6) C13 0.106(8) 0.061(5) 0.095(7) 0.009(5) -0.004(6) 0.031(5) C14 0.083(6) 0.073(5) 0.063(5) -0.023(4) 0.002(4) 0.012(4) #----------------------------------------------------------------------------# # 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 Cd C1 2.210(6) . ? Cd N 2.312(6) . ? Cd Cl 2.5617(14) 3 ? Cd Cl 2.5966(14) . ? Cl Cd 2.5617(14) 3 ? Si1 C1 1.845(6) . ? Si1 C3 1.868(8) . ? Si1 C2 1.879(8) . ? Si1 C4 1.905(7) . ? Si2 C1 1.870(7) . ? Si2 C9 1.873(11) . ? Si2 C11 1.885(12) . ? Si2 C10 1.891(11) . ? Si3 C1 1.869(7) . ? Si3 C12 1.871(10) . ? Si3 C14 1.873(10) . ? Si3 C13 1.879(9) . ? N C8 1.334(9) . ? N C4 1.360(9) . ? C4 C5 1.384(9) . ? C5 C6 1.365(13) . ? C6 C7 1.345(15) . ? C7 C8 1.386(13) . ? 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 C1 Cd N 92.0(2) . . ? C1 Cd Cl 132.08(18) . 3 ? N Cd Cl 105.21(15) . 3 ? C1 Cd Cl 132.42(18) . . ? N Cd Cl 99.32(16) . . ? Cl Cd Cl 89.06(4) 3 . ? Cd Cl Cd 90.94(4) 3 . ? C1 Si1 C3 115.0(4) . . ? C1 Si1 C2 115.9(4) . . ? C3 Si1 C2 107.5(4) . . ? C1 Si1 C4 109.6(3) . . ? C3 Si1 C4 102.0(3) . . ? C2 Si1 C4 105.6(4) . . ? C1 Si1 Cd 44.75(19) . . ? C3 Si1 Cd 101.3(3) . . ? C2 Si1 Cd 150.9(3) . . ? C4 Si1 Cd 71.7(2) . . ? C1 Si2 C9 113.4(3) . . ? C1 Si2 C11 112.4(5) . . ? C9 Si2 C11 104.6(6) . . ? C1 Si2 C10 110.6(4) . . ? C9 Si2 C10 107.8(5) . . ? C11 Si2 C10 107.7(8) . . ? C1 Si2 Cd 37.80(19) . . ? C9 Si2 Cd 82.7(3) . . ? C11 Si2 Cd 101.7(6) . . ? C10 Si2 Cd 144.6(4) . . ? C1 Si3 C12 112.3(4) . . ? C1 Si3 C14 110.7(3) . . ? C12 Si3 C14 106.5(5) . . ? C1 Si3 C13 114.4(4) . . ? C12 Si3 C13 108.1(5) . . ? C14 Si3 C13 104.2(5) . . ? C1 Si3 Cd 42.06(19) . . ? C12 Si3 Cd 153.8(4) . . ? C14 Si3 Cd 91.3(3) . . ? C13 Si3 Cd 85.1(3) . . ? C8 N C4 119.1(7) . . ? C8 N Cd 129.2(6) . . ? C4 N Cd 111.6(4) . . ? Si1 C1 Si3 113.5(3) . . ? Si1 C1 Si2 113.1(4) . . ? Si3 C1 Si2 115.0(3) . . ? Si1 C1 Cd 99.3(3) . . ? Si3 C1 Cd 103.4(3) . . ? Si2 C1 Cd 110.9(3) . . ? N C4 C5 119.2(7) . . ? N C4 Si1 116.3(4) . . ? C5 C4 Si1 124.4(6) . . ? C6 C5 C4 121.1(9) . . ? C7 C6 C5 119.2(8) . . ? C6 C7 C8 119.1(8) . . ? N C8 C7 122.3(9) . . ? #===END data_ce-jds-6 _database_code_CSD 177600 _audit_creation_date 2000-06-26T10:16:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[HgCl{C(SiMe3)2(SiMe2C5H4N)}]' _chemical_formula_moiety 'C14 H28 Cl1 Hg1 N1 Si3' _chemical_formula_structural 'C14 H28 CL HG N SI3' _chemical_formula_sum 'C14 H28 Cl Hg N Si3' _chemical_formula_weight 530.68 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5563(3) _cell_length_b 12.4249(3) _cell_length_c 13.2254(3) _cell_angle_alpha 90 _cell_angle_beta 92.161(2) _cell_angle_gamma 90 _cell_volume 2061.84(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11230 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.71 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.333 _exptl_absorpt_correction_T_max 0.498 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 17731 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 4880 _reflns_number_gt 4353 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0391P)^2^+5.7126P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4880 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.868 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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' 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 Hg Hg 0.912309(10) 0.130374(10) 0.133140(9) 0.02932(6) Uani 1 1 d . . . Cl Cl 0.84535(9) 0.03251(8) -0.00707(7) 0.0430(2) Uani 1 1 d . . . Si1 Si 0.88769(7) 0.22621(9) 0.35310(7) 0.0293(2) Uani 1 1 d . . . Si2 Si 1.11833(8) 0.16491(9) 0.28546(8) 0.0300(2) Uani 1 1 d . . . Si3 Si 0.99304(9) 0.36419(8) 0.18669(9) 0.0353(2) Uani 1 1 d . . . N N 0.7292(2) 0.1793(3) 0.2084(2) 0.0326(7) Uani 1 1 d . . . C1 C 0.9852(3) 0.2272(3) 0.2485(2) 0.0248(7) Uani 1 1 d . . . C2 C 0.9055(4) 0.3421(4) 0.4435(3) 0.0506(11) Uani 1 1 d . . . H2A H 0.8526 0.3372 0.4958 0.076 Uiso 1 1 calc R . . H2B H 0.896 0.41 0.4065 0.076 Uiso 1 1 calc R . . H2C H 0.9773 0.3397 0.4751 0.076 Uiso 1 1 calc R . . C3 C 0.8875(3) 0.0987(4) 0.4288(3) 0.0479(11) Uani 1 1 d . . . H3A H 0.8349 0.1043 0.4814 0.072 Uiso 1 1 calc R . . H3B H 0.9584 0.0871 0.4605 0.072 Uiso 1 1 calc R . . H3C H 0.8693 0.038 0.3841 0.072 Uiso 1 1 calc R . . C4 C 0.7462(3) 0.2338(3) 0.2957(3) 0.0302(7) Uani 1 1 d . . . C5 C 0.6641(3) 0.2868(4) 0.3415(3) 0.0382(9) Uani 1 1 d . . . H5 H 0.6771 0.3244 0.4033 0.046 Uiso 1 1 calc R . . C6 C 0.5616(3) 0.2846(4) 0.2959(4) 0.0465(10) Uani 1 1 d . . . H6 H 0.5043 0.3206 0.3266 0.056 Uiso 1 1 calc R . . C7 C 0.5449(3) 0.2304(4) 0.2073(4) 0.0475(11) Uani 1 1 d . . . H7 H 0.4763 0.2287 0.1745 0.057 Uiso 1 1 calc R . . C8 C 0.6305(3) 0.1777(4) 0.1657(3) 0.0422(10) Uani 1 1 d . . . H8 H 0.6187 0.139 0.1044 0.051 Uiso 1 1 calc R . . C9 C 1.1110(3) 0.0149(3) 0.2907(3) 0.0372(8) Uani 1 1 d . . . H9A H 1.0559 -0.0067 0.3372 0.056 Uiso 1 1 calc R . . H9B H 1.18 -0.014 0.3146 0.056 Uiso 1 1 calc R . . H9C H 1.0931 -0.0134 0.223 0.056 Uiso 1 1 calc R . . C10 C 1.2239(3) 0.1981(4) 0.1939(4) 0.0489(11) Uani 1 1 d . . . H10A H 1.231 0.2765 0.1886 0.073 Uiso 1 1 calc R . . H10B H 1.2038 0.1683 0.1272 0.073 Uiso 1 1 calc R . . H10C H 1.292 0.167 0.2178 0.073 Uiso 1 1 calc R . . C11 C 1.1698(3) 0.2120(4) 0.4132(4) 0.0501(11) Uani 1 1 d . . . H11A H 1.1747 0.2907 0.4135 0.075 Uiso 1 1 calc R . . H11B H 1.2405 0.1811 0.4278 0.075 Uiso 1 1 calc R . . H11C H 1.1209 0.1886 0.465 0.075 Uiso 1 1 calc R . . C12 C 0.8594(3) 0.4303(3) 0.1696(3) 0.0401(9) Uani 1 1 d . . . H12A H 0.8107 0.3823 0.1315 0.06 Uiso 1 1 calc R . . H12B H 0.8669 0.4979 0.1323 0.06 Uiso 1 1 calc R . . H12C H 0.8307 0.4453 0.236 0.06 Uiso 1 1 calc R . . C13 C 1.0823(4) 0.4580(4) 0.2613(5) 0.0580(13) Uani 1 1 d . . . H13A H 1.1528 0.425 0.2717 0.087 Uiso 1 1 calc R . . H13B H 1.0517 0.4723 0.327 0.087 Uiso 1 1 calc R . . H13C H 1.0892 0.5258 0.2241 0.087 Uiso 1 1 calc R . . C14 C 1.0441(5) 0.3543(4) 0.0548(4) 0.0642(16) Uani 1 1 d . . . H14A H 0.9986 0.3052 0.0145 0.096 Uiso 1 1 calc R . . H14B H 1.1173 0.3268 0.0581 0.096 Uiso 1 1 calc R . . H14C H 1.043 0.4257 0.0234 0.096 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 Hg 0.03487(9) 0.03013(9) 0.02276(8) 0.00008(5) -0.00137(6) 0.00078(5) Cl 0.0544(6) 0.0453(5) 0.0285(4) -0.0118(4) -0.0096(4) 0.0027(4) Si1 0.0230(4) 0.0434(6) 0.0217(4) 0.0012(4) 0.0012(3) 0.0024(4) Si2 0.0240(4) 0.0318(5) 0.0342(5) -0.0039(4) 0.0026(4) 0.0014(4) Si3 0.0350(5) 0.0263(5) 0.0455(6) 0.0036(4) 0.0138(5) 0.0013(4) N 0.0298(15) 0.0357(17) 0.0322(16) 0.0059(13) -0.0036(12) -0.0042(13) C1 0.0237(15) 0.0281(17) 0.0227(15) -0.0027(13) 0.0024(12) -0.0015(13) C2 0.036(2) 0.078(3) 0.037(2) -0.018(2) -0.0017(17) 0.006(2) C3 0.036(2) 0.071(3) 0.037(2) 0.023(2) 0.0083(17) 0.007(2) C4 0.0260(16) 0.0371(19) 0.0277(17) 0.0089(15) 0.0023(13) -0.0007(14) C5 0.0303(18) 0.051(2) 0.034(2) 0.0043(17) 0.0072(15) 0.0046(17) C6 0.0280(19) 0.059(3) 0.053(3) 0.015(2) 0.0079(17) 0.0086(18) C7 0.0273(19) 0.062(3) 0.052(3) 0.023(2) -0.0063(17) -0.0023(18) C8 0.035(2) 0.046(2) 0.044(2) 0.0118(19) -0.0110(17) -0.0084(18) C9 0.044(2) 0.0318(19) 0.036(2) 0.0034(16) 0.0031(16) 0.0059(16) C10 0.033(2) 0.042(2) 0.073(3) 0.005(2) 0.019(2) 0.0061(18) C11 0.035(2) 0.061(3) 0.053(3) -0.020(2) -0.0145(19) 0.0067(19) C12 0.041(2) 0.036(2) 0.044(2) 0.0070(17) 0.0074(17) 0.0068(17) C13 0.038(2) 0.036(2) 0.100(4) -0.005(2) 0.009(2) -0.0059(18) C14 0.078(4) 0.053(3) 0.065(3) 0.026(2) 0.044(3) 0.022(3) #----------------------------------------------------------------------------# # 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 Hg C1 2.124(3) . ? Hg Cl 2.3466(9) . ? Hg N 2.611(3) . ? Hg Si3 3.1487(10) . ? Hg Si1 3.1692(10) . ? Si1 C3 1.874(5) . ? Si1 C2 1.880(5) . ? Si1 C1 1.881(3) . ? Si1 C4 1.907(4) . ? Si2 C9 1.868(4) . ? Si2 C10 1.875(4) . ? Si2 C11 1.880(4) . ? Si2 C1 1.890(3) . ? Si3 C13 1.872(5) . ? Si3 C12 1.874(4) . ? Si3 C14 1.884(5) . ? Si3 C1 1.892(4) . ? N C8 1.342(5) . ? N C4 1.349(5) . ? C4 C5 1.381(5) . ? C5 C6 1.401(6) . ? C6 C7 1.361(7) . ? C7 C8 1.390(7) . ? 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 C1 Hg Cl 173.43(9) . . ? C1 Hg N 87.46(11) . . ? Cl Hg N 97.33(7) . . ? C1 Hg Si3 35.83(9) . . ? Cl Hg Si3 139.33(4) . . ? N Hg Si3 88.86(7) . . ? C1 Hg Si1 35.08(9) . . ? Cl Hg Si1 151.12(3) . . ? N Hg Si1 56.27(7) . . ? Si3 Hg Si1 59.24(3) . . ? C3 Si1 C2 108.1(2) . . ? C3 Si1 C1 114.33(18) . . ? C2 Si1 C1 113.40(19) . . ? C3 Si1 C4 103.57(18) . . ? C2 Si1 C4 107.57(19) . . ? C1 Si1 C4 109.24(15) . . ? C3 Si1 Hg 100.06(16) . . ? C2 Si1 Hg 149.11(17) . . ? C1 Si1 Hg 40.45(10) . . ? C4 Si1 Hg 77.01(12) . . ? C9 Si2 C10 106.3(2) . . ? C9 Si2 C11 107.0(2) . . ? C10 Si2 C11 106.6(2) . . ? C9 Si2 C1 111.95(17) . . ? C10 Si2 C1 112.51(18) . . ? C11 Si2 C1 112.05(17) . . ? C13 Si3 C12 107.8(2) . . ? C13 Si3 C14 108.1(3) . . ? C12 Si3 C14 104.6(2) . . ? C13 Si3 C1 111.8(2) . . ? C12 Si3 C1 112.66(17) . . ? C14 Si3 C1 111.50(19) . . ? C13 Si3 Hg 150.96(17) . . ? C12 Si3 Hg 95.63(14) . . ? C14 Si3 Hg 81.35(19) . . ? C1 Si3 Hg 41.06(10) . . ? C8 N C4 118.8(3) . . ? C8 N Hg 130.4(3) . . ? C4 N Hg 109.3(2) . . ? Si1 C1 Si2 113.66(17) . . ? Si1 C1 Si3 111.70(17) . . ? Si2 C1 Si3 114.84(17) . . ? Si1 C1 Hg 104.47(15) . . ? Si2 C1 Hg 107.85(16) . . ? Si3 C1 Hg 103.11(15) . . ? N C4 C5 121.2(3) . . ? N C4 Si1 115.5(3) . . ? C5 C4 Si1 123.3(3) . . ? C4 C5 C6 119.4(4) . . ? C7 C6 C5 119.2(4) . . ? C6 C7 C8 118.6(4) . . ? N C8 C7 122.8(4) . . ? #===END