############################################################################## ### CIF submission form for molecular structure report (Acta Cryst. C) ### ### Version: 2.0.2 (6 July 1998) ### ############################################################################## # This is an electronic "form" for submitting a structural paper to Acta Cryst. # Section C as a Crystallographic Information File. Full details of the format # of such files are given in the paper "The Crystallographic Information File # (CIF): a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # The current version of the core CIF dictionary is obtainable from # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.0.1. # A few data names below appear in the 1998 Notes for Authors [Acta Cryst. # (1998), C54, 153-168] but are not yet in an approved dictionary; these # are indicated by the comment 'Not in version 2.0.1'. # # Note that all fields should be numeric or character type EXCEPT those which # are flagged as 'text' - free-form text of any length may be included in # these latter fields provided the text block begins and ends with a semicolon # as the first character of a new line. Note also that the query marks # '?' are significant as placeholders, and should not be deleted where a data # item is not given, UNLESS the accompanying data name is also deleted. # Lines should not exceed 80 characters in length. # # An example file derived from this form and annotated in the 1998 Notes for # Authors may be retrieved as ftp://ftp.iucr.org/pub/example.cif. #============================================================================== data_? _publ_requested_journal Organometallics #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Dr. Frank Breher' _publ_contact_author_address ; Institute of Inorganic Chemistry Karlsruhe Institute of Technology (KIT) Engesserstr. 15 76131 Karlsruhe Germany ; _publ_contact_author_email breher@kit.edu _publ_contact_author_phone ? _publ_contact_author_fax '(+49) 721 608 70 21' loop_ _publ_author_name _publ_author_address 'Nied, Dominik' ; Institute of Inorganic Chemistry Karlsruhe Institute of Technology Engesserstr. 15 76131 Karlsruhe Germany ; 'Burgos, Pascual Ona' ; Institute of Inorganic Chemistry Karlsruhe Institute of Technology Engesserstr. 15 76131 Karlsruhe Germany ; 'Klopper, Wim' ; Institute of Physical Chemistry Karlsruhe Institute of Technology Fritz-Haber-Weg 2 76131 Karlsruhe Germany ; 'Breher, Frank' ; Institute of Inorganic Chemistry Karlsruhe Institute of Technology Engesserstr. 15 76131 Karlsruhe Germany ; #============================================================================== _audit_creation_method 'form.cif (version 2.0)' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _publ_contact_letter ; ? ; _publ_requested_category FA #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Tuning the Gap: Electronic Properties and Radical-Type Reactivities of Heteronuclear [1.1.1]Propellanes of Heavier Group 14 Elements ; _publ_section_title_footnote ; ? ; #============================================================================== # TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_1 _chemical_name_systematic ; Ge2Si3Mes6 ; _publ_section_exptl_refinement ; ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H66 Ge2 Si3' _chemical_formula_sum 'C54 H66 Ge2 Si3' _chemical_formula_weight 944.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.4970(17) _cell_length_b 26.976(5) _cell_length_c 41.646(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9546(3) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 65167 _cell_measurement_theta_min 3.84 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 1.370 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65167 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9368 _reflns_number_gt 7589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+12.5289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9368 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.001 _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 Ge1 Ge 0.43547(5) 0.396915(15) 0.607994(10) 0.02693(12) Uani 1 1 d . . . Si1 Si 0.51790(13) 0.38038(4) 0.66252(3) 0.0267(2) Uani 1 1 d . . . Ge2 Ge 0.72856(5) 0.361138(15) 0.625378(10) 0.02744(13) Uani 1 1 d . . . Si2 Si 0.68410(13) 0.43789(4) 0.59702(3) 0.0282(3) Uani 1 1 d . . . Si3 Si 0.54041(12) 0.31884(4) 0.59064(3) 0.0249(2) Uani 1 1 d . . . C100 C 0.4282(5) 0.32536(14) 0.68423(9) 0.0268(8) Uani 1 1 d . . . C101 C 0.2708(5) 0.32939(16) 0.69459(10) 0.0328(9) Uani 1 1 d . . . C102 C 0.1968(6) 0.28899(16) 0.70908(11) 0.0386(10) Uani 1 1 d . . . H10A H 0.0905 0.2923 0.7159 0.046 Uiso 1 1 calc R . . C103 C 0.2730(6) 0.24449(17) 0.71385(11) 0.0414(11) Uani 1 1 d . . . C104 C 0.4271(6) 0.24150(15) 0.70455(10) 0.0362(10) Uani 1 1 d . . . H10B H 0.4818 0.2113 0.7081 0.043 Uiso 1 1 calc R . . C105 C 0.5072(5) 0.28041(15) 0.69023(10) 0.0320(9) Uani 1 1 d . . . C106 C 0.1753(5) 0.37566(16) 0.68961(12) 0.0393(10) Uani 1 1 d . . . H10C H 0.0783 0.3736 0.7022 0.059 Uiso 1 1 calc R . . H10D H 0.1490 0.3790 0.6668 0.059 Uiso 1 1 calc R . . H10E H 0.2365 0.4045 0.6965 0.059 Uiso 1 1 calc R . . C107 C 0.1879(7) 0.20067(19) 0.72779(14) 0.0641(16) Uani 1 1 d . . . H10F H 0.1957 0.1726 0.7130 0.096 Uiso 1 1 calc R . . H10G H 0.0769 0.2091 0.7311 0.096 Uiso 1 1 calc R . . H10H H 0.2357 0.1917 0.7484 0.096 Uiso 1 1 calc R . . C108 C 0.6760(5) 0.27087(15) 0.68202(11) 0.0371(10) Uani 1 1 d . . . H10I H 0.7374 0.3012 0.6855 0.056 Uiso 1 1 calc R . . H10J H 0.6840 0.2609 0.6595 0.056 Uiso 1 1 calc R . . H10K H 0.7170 0.2443 0.6957 0.056 Uiso 1 1 calc R . . C200 C 0.5342(5) 0.43603(14) 0.69032(10) 0.0272(9) Uani 1 1 d . . . C201 C 0.4514(5) 0.48089(14) 0.68577(10) 0.0290(9) Uani 1 1 d . . . C202 C 0.4741(5) 0.51955(15) 0.70731(11) 0.0357(10) Uani 1 1 d . . . H20A H 0.4191 0.5497 0.7038 0.043 Uiso 1 1 calc R . . C203 C 0.5716(5) 0.51629(16) 0.73330(11) 0.0379(10) Uani 1 1 d . . . C204 C 0.6506(5) 0.47203(16) 0.73802(11) 0.0379(10) Uani 1 1 d . . . H20B H 0.7188 0.4688 0.7560 0.046 Uiso 1 1 calc R . . C205 C 0.6330(5) 0.43235(15) 0.71736(10) 0.0322(9) Uani 1 1 d . . . C206 C 0.3396(5) 0.49058(16) 0.65876(11) 0.0373(10) Uani 1 1 d . . . H20C H 0.2708 0.5184 0.6644 0.056 Uiso 1 1 calc R . . H20D H 0.2756 0.4610 0.6549 0.056 Uiso 1 1 calc R . . H20E H 0.3991 0.4987 0.6393 0.056 Uiso 1 1 calc R . . C207 C 0.5952(7) 0.55995(18) 0.75555(14) 0.0563(14) Uani 1 1 d . . . H20F H 0.5032 0.5818 0.7544 0.084 Uiso 1 1 calc R . . H20G H 0.6893 0.5784 0.7490 0.084 Uiso 1 1 calc R . . H20H H 0.6085 0.5480 0.7776 0.084 Uiso 1 1 calc R . . C208 C 0.7254(5) 0.38576(16) 0.72433(11) 0.0386(11) Uani 1 1 d . . . H20I H 0.8021 0.3924 0.7414 0.058 Uiso 1 1 calc R . . H20J H 0.7807 0.3752 0.7049 0.058 Uiso 1 1 calc R . . H20K H 0.6533 0.3595 0.7313 0.058 Uiso 1 1 calc R . . C300 C 0.7154(5) 0.49866(15) 0.61922(10) 0.0307(9) Uani 1 1 d . . . C301 C 0.6325(5) 0.54066(15) 0.60799(11) 0.0339(10) Uani 1 1 d . . . C302 C 0.6373(6) 0.58460(16) 0.62543(12) 0.0409(11) Uani 1 1 d . . . H30A H 0.5811 0.6125 0.6175 0.049 Uiso 1 1 calc R . . C303 C 0.7195(6) 0.58950(17) 0.65349(12) 0.0410(11) Uani 1 1 d . . . C304 C 0.8051(5) 0.54933(17) 0.66323(11) 0.0417(11) Uani 1 1 d . . . H30B H 0.8674 0.5524 0.6821 0.050 Uiso 1 1 calc R . . C305 C 0.8063(5) 0.50421(16) 0.64713(11) 0.0339(10) Uani 1 1 d . . . C306 C 0.5363(6) 0.53945(17) 0.57796(12) 0.0478(13) Uani 1 1 d . . . H30C H 0.4912 0.5723 0.5740 0.072 Uiso 1 1 calc R . . H30D H 0.4513 0.5152 0.5803 0.072 Uiso 1 1 calc R . . H30E H 0.6033 0.5300 0.5598 0.072 Uiso 1 1 calc R . . C307 C 0.7143(7) 0.63619(19) 0.67300(15) 0.0630(16) Uani 1 1 d . . . H30F H 0.8114 0.6392 0.6855 0.095 Uiso 1 1 calc R . . H30G H 0.6237 0.6351 0.6876 0.095 Uiso 1 1 calc R . . H30H H 0.7043 0.6648 0.6586 0.095 Uiso 1 1 calc R . . C308 C 0.9075(5) 0.46361(17) 0.66069(11) 0.0414(11) Uani 1 1 d . . . H30I H 0.9527 0.4745 0.6812 0.062 Uiso 1 1 calc R . . H30J H 0.9924 0.4560 0.6456 0.062 Uiso 1 1 calc R . . H30K H 0.8433 0.4339 0.6642 0.062 Uiso 1 1 calc R . . C400 C 0.7623(5) 0.44065(14) 0.55439(10) 0.0315(9) Uani 1 1 d . . . C401 C 0.6697(5) 0.43860(15) 0.52614(10) 0.0349(10) Uani 1 1 d . . . C402 C 0.7425(6) 0.43661(17) 0.49641(12) 0.0446(12) Uani 1 1 d . . . H40A H 0.6787 0.4361 0.4777 0.053 Uiso 1 1 calc R . . C403 C 0.9033(7) 0.43534(17) 0.49290(12) 0.0499(13) Uani 1 1 d . . . C404 C 0.9932(6) 0.43882(17) 0.52028(13) 0.0462(12) Uani 1 1 d . . . H40B H 1.1045 0.4394 0.5183 0.055 Uiso 1 1 calc R . . C405 C 0.9269(5) 0.44153(16) 0.55073(12) 0.0401(11) Uani 1 1 d . . . C406 C 0.4939(5) 0.43888(16) 0.52620(11) 0.0387(11) Uani 1 1 d . . . H40C H 0.4549 0.4183 0.5085 0.058 Uiso 1 1 calc R . . H40D H 0.4559 0.4729 0.5235 0.058 Uiso 1 1 calc R . . H40E H 0.4554 0.4256 0.5466 0.058 Uiso 1 1 calc R . . C407 C 0.9788(8) 0.4291(2) 0.46039(14) 0.0725(19) Uani 1 1 d . . . H40F H 0.9035 0.4384 0.4436 0.109 Uiso 1 1 calc R . . H40G H 1.0101 0.3944 0.4575 0.109 Uiso 1 1 calc R . . H40H H 1.0719 0.4504 0.4589 0.109 Uiso 1 1 calc R . . C408 C 1.0350(5) 0.4452(2) 0.57885(13) 0.0489(13) Uani 1 1 d . . . H40I H 1.1435 0.4492 0.5713 0.073 Uiso 1 1 calc R . . H40J H 1.0270 0.4150 0.5918 0.073 Uiso 1 1 calc R . . H40K H 1.0056 0.4740 0.5920 0.073 Uiso 1 1 calc R . . C500 C 0.5853(4) 0.31396(13) 0.54630(9) 0.0244(8) Uani 1 1 d . . . C501 C 0.4561(5) 0.31315(14) 0.52502(10) 0.0282(9) Uani 1 1 d . . . C502 C 0.4807(5) 0.31296(15) 0.49211(10) 0.0334(10) Uani 1 1 d . . . H50A H 0.3921 0.3125 0.4782 0.040 Uiso 1 1 calc R . . C503 C 0.6288(5) 0.31342(15) 0.47893(10) 0.0341(10) Uani 1 1 d . . . C504 C 0.7546(5) 0.31176(15) 0.49985(10) 0.0338(10) Uani 1 1 d . . . H50B H 0.8580 0.3098 0.4913 0.041 Uiso 1 1 calc R . . C505 C 0.7362(5) 0.31279(14) 0.53278(10) 0.0277(9) Uani 1 1 d . . . C506 C 0.2884(5) 0.31400(17) 0.53651(11) 0.0357(10) Uani 1 1 d . . . H50C H 0.2174 0.3107 0.5181 0.054 Uiso 1 1 calc R . . H50D H 0.2675 0.3454 0.5475 0.054 Uiso 1 1 calc R . . H50E H 0.2709 0.2864 0.5514 0.054 Uiso 1 1 calc R . . C507 C 0.6528(6) 0.31616(19) 0.44328(11) 0.0463(12) Uani 1 1 d . . . H50F H 0.5834 0.2922 0.4326 0.069 Uiso 1 1 calc R . . H50G H 0.7626 0.3084 0.4382 0.069 Uiso 1 1 calc R . . H50H H 0.6279 0.3497 0.4357 0.069 Uiso 1 1 calc R . . C508 C 0.8864(5) 0.31255(16) 0.55214(11) 0.0353(10) Uani 1 1 d . . . H50I H 0.9477 0.2829 0.5469 0.053 Uiso 1 1 calc R . . H50J H 0.8608 0.3125 0.5751 0.053 Uiso 1 1 calc R . . H50K H 0.9482 0.3422 0.5470 0.053 Uiso 1 1 calc R . . C600 C 0.4511(5) 0.25925(14) 0.60643(9) 0.0254(8) Uani 1 1 d . . . C601 C 0.2982(5) 0.25470(15) 0.61956(10) 0.0290(9) Uani 1 1 d . . . C602 C 0.2497(5) 0.20943(17) 0.63240(10) 0.0366(10) Uani 1 1 d . . . H60A H 0.1483 0.2073 0.6419 0.044 Uiso 1 1 calc R . . C603 C 0.3431(6) 0.16796(17) 0.63181(11) 0.0419(11) Uani 1 1 d . . . C604 C 0.4883(6) 0.17161(16) 0.61764(11) 0.0409(11) Uani 1 1 d . . . H60B H 0.5521 0.1428 0.6161 0.049 Uiso 1 1 calc R . . C605 C 0.5448(5) 0.21597(15) 0.60553(10) 0.0310(9) Uani 1 1 d . . . C607 C 0.1791(5) 0.29564(16) 0.61957(10) 0.0333(10) Uani 1 1 d . . . H60C H 0.0887 0.2860 0.6328 0.050 Uiso 1 1 calc R . . H60D H 0.1440 0.3019 0.5975 0.050 Uiso 1 1 calc R . . H60E H 0.2267 0.3258 0.6284 0.050 Uiso 1 1 calc R . . C608 C 0.2896(7) 0.11963(19) 0.64588(16) 0.0623(16) Uani 1 1 d . . . H60F H 0.1855 0.1239 0.6556 0.093 Uiso 1 1 calc R . . H60G H 0.3647 0.1089 0.6623 0.093 Uiso 1 1 calc R . . H60H H 0.2837 0.0946 0.6289 0.093 Uiso 1 1 calc R . . C609 C 0.7068(5) 0.21615(17) 0.59134(12) 0.0435(11) Uani 1 1 d . . . H60I H 0.7510 0.1826 0.5923 0.065 Uiso 1 1 calc R . . H60J H 0.7740 0.2389 0.6035 0.065 Uiso 1 1 calc R . . H60K H 0.7013 0.2270 0.5689 0.065 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 Ge1 0.0252(2) 0.0265(2) 0.0291(2) 0.00130(18) -0.00206(18) 0.00200(17) Si1 0.0280(6) 0.0253(5) 0.0268(6) 0.0001(4) -0.0014(5) 0.0028(4) Ge2 0.0250(2) 0.0268(2) 0.0305(2) 0.00143(18) -0.00216(18) 0.00111(17) Si2 0.0273(6) 0.0254(5) 0.0318(6) 0.0040(5) -0.0038(5) -0.0015(4) Si3 0.0231(5) 0.0262(5) 0.0256(6) 0.0003(4) 0.0010(4) -0.0007(4) C100 0.034(2) 0.0262(19) 0.021(2) -0.0012(16) -0.0025(17) 0.0003(17) C101 0.036(2) 0.034(2) 0.028(2) -0.0029(18) 0.0013(18) 0.0034(18) C102 0.042(3) 0.041(2) 0.033(2) -0.002(2) 0.009(2) -0.005(2) C103 0.062(3) 0.034(2) 0.029(2) 0.0008(19) 0.005(2) -0.004(2) C104 0.050(3) 0.028(2) 0.030(2) 0.0028(18) -0.002(2) 0.001(2) C105 0.040(2) 0.029(2) 0.027(2) -0.0021(17) -0.0047(19) 0.0062(19) C106 0.034(2) 0.038(2) 0.045(3) 0.002(2) 0.006(2) 0.005(2) C107 0.087(4) 0.043(3) 0.062(4) 0.008(3) 0.018(3) -0.013(3) C108 0.041(3) 0.028(2) 0.042(3) 0.0053(19) -0.005(2) 0.0104(19) C200 0.027(2) 0.025(2) 0.029(2) 0.0005(16) 0.0026(17) 0.0026(16) C201 0.026(2) 0.029(2) 0.032(2) 0.0020(17) 0.0063(17) 0.0006(17) C202 0.038(2) 0.028(2) 0.041(3) -0.0068(19) 0.007(2) -0.0004(18) C203 0.041(3) 0.035(2) 0.038(2) -0.010(2) 0.009(2) -0.006(2) C204 0.041(3) 0.042(3) 0.031(2) -0.0062(19) -0.003(2) -0.002(2) C205 0.032(2) 0.035(2) 0.029(2) 0.0002(18) 0.0015(18) 0.0012(18) C206 0.033(2) 0.030(2) 0.048(3) 0.001(2) -0.002(2) 0.0045(19) C207 0.061(3) 0.050(3) 0.059(3) -0.022(3) -0.001(3) -0.002(3) C208 0.046(3) 0.038(2) 0.032(2) -0.0027(19) -0.010(2) 0.006(2) C300 0.027(2) 0.029(2) 0.036(2) 0.0008(18) -0.0027(18) -0.0026(17) C301 0.034(2) 0.023(2) 0.045(3) 0.0020(19) 0.003(2) -0.0047(17) C302 0.043(3) 0.029(2) 0.051(3) 0.003(2) 0.009(2) 0.000(2) C303 0.042(3) 0.033(2) 0.048(3) -0.006(2) 0.008(2) -0.011(2) C304 0.037(3) 0.048(3) 0.041(3) -0.012(2) 0.000(2) -0.017(2) C305 0.025(2) 0.037(2) 0.040(2) 0.0050(19) 0.0002(18) -0.0099(18) C306 0.061(3) 0.030(2) 0.052(3) 0.003(2) -0.013(3) 0.010(2) C307 0.081(4) 0.042(3) 0.066(4) -0.022(3) 0.006(3) -0.006(3) C308 0.033(2) 0.049(3) 0.042(3) 0.003(2) -0.009(2) -0.005(2) C400 0.034(2) 0.0236(19) 0.037(2) 0.0067(17) 0.0049(19) 0.0007(17) C401 0.047(3) 0.027(2) 0.031(2) 0.0051(18) 0.000(2) 0.0003(19) C402 0.065(3) 0.034(2) 0.035(3) 0.005(2) -0.001(2) 0.002(2) C403 0.074(4) 0.032(2) 0.044(3) 0.004(2) 0.019(3) -0.003(2) C404 0.044(3) 0.040(3) 0.055(3) 0.006(2) 0.017(2) 0.000(2) C405 0.038(2) 0.030(2) 0.052(3) 0.005(2) 0.010(2) -0.0003(19) C406 0.047(3) 0.032(2) 0.037(3) 0.0049(19) -0.010(2) -0.002(2) C407 0.103(5) 0.058(4) 0.057(4) -0.001(3) 0.037(4) -0.007(3) C408 0.027(2) 0.060(3) 0.060(3) 0.012(3) 0.000(2) -0.007(2) C500 0.026(2) 0.0212(18) 0.026(2) -0.0005(15) 0.0035(16) 0.0038(15) C501 0.027(2) 0.028(2) 0.029(2) -0.0017(17) 0.0013(17) -0.0022(17) C502 0.037(2) 0.033(2) 0.030(2) 0.0005(18) -0.0023(19) 0.0000(19) C503 0.042(2) 0.031(2) 0.029(2) 0.0007(18) 0.005(2) 0.0031(19) C504 0.034(2) 0.029(2) 0.038(2) 0.0010(18) 0.011(2) 0.0028(18) C505 0.029(2) 0.0247(19) 0.030(2) -0.0003(16) 0.0038(17) 0.0019(16) C506 0.022(2) 0.051(3) 0.034(2) -0.003(2) 0.0000(18) -0.0043(19) C507 0.056(3) 0.052(3) 0.031(2) 0.004(2) 0.007(2) 0.007(2) C508 0.024(2) 0.039(2) 0.043(3) 0.002(2) 0.0050(19) 0.0033(18) C600 0.027(2) 0.029(2) 0.021(2) -0.0002(16) -0.0055(16) -0.0034(16) C601 0.026(2) 0.036(2) 0.026(2) -0.0007(17) -0.0027(17) -0.0048(17) C602 0.038(2) 0.042(2) 0.030(2) 0.0051(19) -0.0030(19) -0.015(2) C603 0.046(3) 0.039(3) 0.041(3) 0.011(2) -0.011(2) -0.012(2) C604 0.047(3) 0.031(2) 0.045(3) 0.002(2) -0.011(2) 0.001(2) C605 0.032(2) 0.030(2) 0.031(2) -0.0011(18) -0.0011(18) 0.0026(17) C607 0.025(2) 0.044(2) 0.031(2) -0.0018(19) 0.0035(18) -0.0047(19) C608 0.063(4) 0.044(3) 0.080(4) 0.027(3) -0.005(3) -0.013(3) C609 0.040(3) 0.035(2) 0.056(3) 0.009(2) 0.008(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 Si3 2.3987(12) . ? Ge1 Si1 2.4179(13) . ? Ge1 Si2 2.4277(13) . ? Ge1 Ge2 2.7672(7) . ? Si1 C100 1.898(4) . ? Si1 C200 1.901(4) . ? Si1 Ge2 2.4219(12) . ? Ge2 Si2 2.4132(12) . ? Ge2 Si3 2.4394(12) . ? Si2 C400 1.897(4) . ? Si2 C300 1.901(4) . ? Si3 C500 1.890(4) . ? Si3 C600 1.895(4) . ? C100 C105 1.408(5) . ? C100 C101 1.409(6) . ? C101 C102 1.396(6) . ? C101 C106 1.503(6) . ? C102 C103 1.378(6) . ? C102 H10A 0.9500 . ? C103 C104 1.368(7) . ? C103 C107 1.502(6) . ? C104 C105 1.386(6) . ? C104 H10B 0.9500 . ? C105 C108 1.497(6) . ? C106 H10C 0.9800 . ? C106 H10D 0.9800 . ? C106 H10E 0.9800 . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? C107 H10H 0.9800 . ? C108 H10I 0.9800 . ? C108 H10J 0.9800 . ? C108 H10K 0.9800 . ? C200 C205 1.408(6) . ? C200 C201 1.413(5) . ? C201 C202 1.389(6) . ? C201 C206 1.495(6) . ? C202 C203 1.366(6) . ? C202 H20A 0.9500 . ? C203 C204 1.384(6) . ? C203 C207 1.512(6) . ? C204 C205 1.381(6) . ? C204 H20B 0.9500 . ? C205 C208 1.510(6) . ? C206 H20C 0.9800 . ? C206 H20D 0.9800 . ? C206 H20E 0.9800 . ? C207 H20F 0.9800 . ? C207 H20G 0.9800 . ? C207 H20H 0.9800 . ? C208 H20I 0.9800 . ? C208 H20J 0.9800 . ? C208 H20K 0.9800 . ? C300 C305 1.404(6) . ? C300 C301 1.414(6) . ? C301 C302 1.391(6) . ? C301 C306 1.495(6) . ? C302 C303 1.368(7) . ? C302 H30A 0.9500 . ? C303 C304 1.367(7) . ? C303 C307 1.499(6) . ? C304 C305 1.390(6) . ? C304 H30B 0.9500 . ? C305 C308 1.503(6) . ? C306 H30C 0.9800 . ? C306 H30D 0.9800 . ? C306 H30E 0.9800 . ? C307 H30F 0.9800 . ? C307 H30G 0.9800 . ? C307 H30H 0.9800 . ? C308 H30I 0.9800 . ? C308 H30J 0.9800 . ? C308 H30K 0.9800 . ? C400 C405 1.407(6) . ? C400 C401 1.416(6) . ? C401 C402 1.385(6) . ? C401 C406 1.494(6) . ? C402 C403 1.375(7) . ? C402 H40A 0.9500 . ? C403 C404 1.375(7) . ? C403 C407 1.508(7) . ? C404 C405 1.389(7) . ? C404 H40B 0.9500 . ? C405 C408 1.491(7) . ? C406 H40C 0.9800 . ? C406 H40D 0.9800 . ? C406 H40E 0.9800 . ? C407 H40F 0.9800 . ? C407 H40G 0.9800 . ? C407 H40H 0.9800 . ? C408 H40I 0.9800 . ? C408 H40J 0.9800 . ? C408 H40K 0.9800 . ? C500 C505 1.401(5) . ? C500 C501 1.411(5) . ? C501 C502 1.387(6) . ? C501 C506 1.504(5) . ? C502 C503 1.373(6) . ? C502 H50A 0.9500 . ? C503 C504 1.380(6) . ? C503 C507 1.501(6) . ? C504 C505 1.380(6) . ? C504 H50B 0.9500 . ? C505 C508 1.510(6) . ? C506 H50C 0.9800 . ? C506 H50D 0.9800 . ? C506 H50E 0.9800 . ? C507 H50F 0.9800 . ? C507 H50G 0.9800 . ? C507 H50H 0.9800 . ? C508 H50I 0.9800 . ? C508 H50J 0.9800 . ? C508 H50K 0.9800 . ? C600 C605 1.414(5) . ? C600 C601 1.415(5) . ? C601 C602 1.395(6) . ? C601 C607 1.498(6) . ? C602 C603 1.372(7) . ? C602 H60A 0.9500 . ? C603 C604 1.371(7) . ? C603 C608 1.500(6) . ? C604 C605 1.385(6) . ? C604 H60B 0.9500 . ? C605 C609 1.498(6) . ? C607 H60C 0.9800 . ? C607 H60D 0.9800 . ? C607 H60E 0.9800 . ? C608 H60F 0.9800 . ? C608 H60G 0.9800 . ? C608 H60H 0.9800 . ? C609 H60I 0.9800 . ? C609 H60J 0.9800 . ? C609 H60K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si3 Ge1 Si1 90.76(4) . . ? Si3 Ge1 Si2 91.12(4) . . ? Si1 Ge1 Si2 90.49(4) . . ? Si3 Ge1 Ge2 55.81(3) . . ? Si1 Ge1 Ge2 55.20(3) . . ? Si2 Ge1 Ge2 54.89(3) . . ? C100 Si1 C200 110.90(17) . . ? C100 Si1 Ge1 118.39(13) . . ? C200 Si1 Ge1 116.58(13) . . ? C100 Si1 Ge2 115.69(13) . . ? C200 Si1 Ge2 120.28(13) . . ? Ge1 Si1 Ge2 69.75(4) . . ? Si2 Ge2 Si1 90.74(4) . . ? Si2 Ge2 Si3 90.49(4) . . ? Si1 Ge2 Si3 89.69(4) . . ? Si2 Ge2 Ge1 55.38(3) . . ? Si1 Ge2 Ge1 55.06(3) . . ? Si3 Ge2 Ge1 54.42(3) . . ? C400 Si2 C300 111.85(18) . . ? C400 Si2 Ge2 115.90(13) . . ? C300 Si2 Ge2 118.70(14) . . ? C400 Si2 Ge1 119.92(14) . . ? C300 Si2 Ge1 115.02(14) . . ? Ge2 Si2 Ge1 69.73(3) . . ? C500 Si3 C600 111.14(17) . . ? C500 Si3 Ge1 115.49(12) . . ? C600 Si3 Ge1 119.43(13) . . ? C500 Si3 Ge2 118.67(13) . . ? C600 Si3 Ge2 116.97(12) . . ? Ge1 Si3 Ge2 69.77(3) . . ? C105 C100 C101 117.7(4) . . ? C105 C100 Si1 124.5(3) . . ? C101 C100 Si1 117.8(3) . . ? C102 C101 C100 120.0(4) . . ? C102 C101 C106 117.7(4) . . ? C100 C101 C106 122.3(4) . . ? C103 C102 C101 122.0(4) . . ? C103 C102 H10A 119.0 . . ? C101 C102 H10A 119.0 . . ? C104 C103 C102 117.4(4) . . ? C104 C103 C107 121.6(5) . . ? C102 C103 C107 121.0(5) . . ? C103 C104 C105 123.2(4) . . ? C103 C104 H10B 118.4 . . ? C105 C104 H10B 118.4 . . ? C104 C105 C100 119.6(4) . . ? C104 C105 C108 116.0(4) . . ? C100 C105 C108 124.3(4) . . ? C101 C106 H10C 109.5 . . ? C101 C106 H10D 109.5 . . ? H10C C106 H10D 109.5 . . ? C101 C106 H10E 109.5 . . ? H10C C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C103 C107 H10F 109.5 . . ? C103 C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C103 C107 H10H 109.5 . . ? H10F C107 H10H 109.5 . . ? H10G C107 H10H 109.5 . . ? C105 C108 H10I 109.5 . . ? C105 C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? C105 C108 H10K 109.5 . . ? H10I C108 H10K 109.5 . . ? H10J C108 H10K 109.5 . . ? C205 C200 C201 117.7(4) . . ? C205 C200 Si1 118.4(3) . . ? C201 C200 Si1 123.9(3) . . ? C202 C201 C200 119.2(4) . . ? C202 C201 C206 116.3(4) . . ? C200 C201 C206 124.6(4) . . ? C203 C202 C201 123.2(4) . . ? C203 C202 H20A 118.4 . . ? C201 C202 H20A 118.4 . . ? C202 C203 C204 117.5(4) . . ? C202 C203 C207 121.1(4) . . ? C204 C203 C207 121.4(4) . . ? C205 C204 C203 121.9(4) . . ? C205 C204 H20B 119.1 . . ? C203 C204 H20B 119.1 . . ? C204 C205 C200 120.5(4) . . ? C204 C205 C208 118.0(4) . . ? C200 C205 C208 121.5(4) . . ? C201 C206 H20C 109.5 . . ? C201 C206 H20D 109.5 . . ? H20C C206 H20D 109.5 . . ? C201 C206 H20E 109.5 . . ? H20C C206 H20E 109.5 . . ? H20D C206 H20E 109.5 . . ? C203 C207 H20F 109.5 . . ? C203 C207 H20G 109.5 . . ? H20F C207 H20G 109.5 . . ? C203 C207 H20H 109.5 . . ? H20F C207 H20H 109.5 . . ? H20G C207 H20H 109.5 . . ? C205 C208 H20I 109.5 . . ? C205 C208 H20J 109.5 . . ? H20I C208 H20J 109.5 . . ? C205 C208 H20K 109.5 . . ? H20I C208 H20K 109.5 . . ? H20J C208 H20K 109.5 . . ? C305 C300 C301 117.6(4) . . ? C305 C300 Si2 124.9(3) . . ? C301 C300 Si2 117.4(3) . . ? C302 C301 C300 119.7(4) . . ? C302 C301 C306 118.1(4) . . ? C300 C301 C306 122.1(4) . . ? C303 C302 C301 122.9(4) . . ? C303 C302 H30A 118.5 . . ? C301 C302 H30A 118.5 . . ? C304 C303 C302 116.7(4) . . ? C304 C303 C307 121.4(5) . . ? C302 C303 C307 121.9(5) . . ? C303 C304 C305 123.7(4) . . ? C303 C304 H30B 118.1 . . ? C305 C304 H30B 118.1 . . ? C304 C305 C300 119.3(4) . . ? C304 C305 C308 117.4(4) . . ? C300 C305 C308 123.3(4) . . ? C301 C306 H30C 109.5 . . ? C301 C306 H30D 109.5 . . ? H30C C306 H30D 109.5 . . ? C301 C306 H30E 109.5 . . ? H30C C306 H30E 109.5 . . ? H30D C306 H30E 109.5 . . ? C303 C307 H30F 109.5 . . ? C303 C307 H30G 109.5 . . ? H30F C307 H30G 109.5 . . ? C303 C307 H30H 109.5 . . ? H30F C307 H30H 109.5 . . ? H30G C307 H30H 109.5 . . ? C305 C308 H30I 109.5 . . ? C305 C308 H30J 109.5 . . ? H30I C308 H30J 109.5 . . ? C305 C308 H30K 109.5 . . ? H30I C308 H30K 109.5 . . ? H30J C308 H30K 109.5 . . ? C405 C400 C401 117.6(4) . . ? C405 C400 Si2 116.7(3) . . ? C401 C400 Si2 125.5(3) . . ? C402 C401 C400 119.7(4) . . ? C402 C401 C406 116.6(4) . . ? C400 C401 C406 123.6(4) . . ? C403 C402 C401 122.7(5) . . ? C403 C402 H40A 118.7 . . ? C401 C402 H40A 118.7 . . ? C402 C403 C404 117.5(5) . . ? C402 C403 C407 121.4(6) . . ? C404 C403 C407 121.1(5) . . ? C403 C404 C405 122.4(5) . . ? C403 C404 H40B 118.8 . . ? C405 C404 H40B 118.8 . . ? C404 C405 C400 120.0(5) . . ? C404 C405 C408 118.1(4) . . ? C400 C405 C408 121.9(4) . . ? C401 C406 H40C 109.5 . . ? C401 C406 H40D 109.5 . . ? H40C C406 H40D 109.5 . . ? C401 C406 H40E 109.5 . . ? H40C C406 H40E 109.5 . . ? H40D C406 H40E 109.5 . . ? C403 C407 H40F 109.5 . . ? C403 C407 H40G 109.5 . . ? H40F C407 H40G 109.5 . . ? C403 C407 H40H 109.5 . . ? H40F C407 H40H 109.5 . . ? H40G C407 H40H 109.5 . . ? C405 C408 H40I 109.5 . . ? C405 C408 H40J 109.5 . . ? H40I C408 H40J 109.5 . . ? C405 C408 H40K 109.5 . . ? H40I C408 H40K 109.5 . . ? H40J C408 H40K 109.5 . . ? C505 C500 C501 117.3(4) . . ? C505 C500 Si3 125.4(3) . . ? C501 C500 Si3 117.3(3) . . ? C502 C501 C500 120.3(4) . . ? C502 C501 C506 117.2(4) . . ? C500 C501 C506 122.5(4) . . ? C503 C502 C501 122.2(4) . . ? C503 C502 H50A 118.9 . . ? C501 C502 H50A 118.9 . . ? C502 C503 C504 117.2(4) . . ? C502 C503 C507 121.3(4) . . ? C504 C503 C507 121.4(4) . . ? C503 C504 C505 122.6(4) . . ? C503 C504 H50B 118.7 . . ? C505 C504 H50B 118.7 . . ? C504 C505 C500 120.2(4) . . ? C504 C505 C508 115.8(4) . . ? C500 C505 C508 124.0(4) . . ? C501 C506 H50C 109.5 . . ? C501 C506 H50D 109.5 . . ? H50C C506 H50D 109.5 . . ? C501 C506 H50E 109.5 . . ? H50C C506 H50E 109.5 . . ? H50D C506 H50E 109.5 . . ? C503 C507 H50F 109.5 . . ? C503 C507 H50G 109.5 . . ? H50F C507 H50G 109.5 . . ? C503 C507 H50H 109.5 . . ? H50F C507 H50H 109.5 . . ? H50G C507 H50H 109.5 . . ? C505 C508 H50I 109.5 . . ? C505 C508 H50J 109.5 . . ? H50I C508 H50J 109.5 . . ? C505 C508 H50K 109.5 . . ? H50I C508 H50K 109.5 . . ? H50J C508 H50K 109.5 . . ? C605 C600 C601 117.1(4) . . ? C605 C600 Si3 117.8(3) . . ? C601 C600 Si3 125.1(3) . . ? C602 C601 C600 119.7(4) . . ? C602 C601 C607 116.5(4) . . ? C600 C601 C607 123.8(4) . . ? C603 C602 C601 122.4(4) . . ? C603 C602 H60A 118.8 . . ? C601 C602 H60A 118.8 . . ? C604 C603 C602 118.0(4) . . ? C604 C603 C608 120.2(5) . . ? C602 C603 C608 121.8(5) . . ? C603 C604 C605 122.1(4) . . ? C603 C604 H60B 119.0 . . ? C605 C604 H60B 119.0 . . ? C604 C605 C600 120.6(4) . . ? C604 C605 C609 117.7(4) . . ? C600 C605 C609 121.7(4) . . ? C601 C607 H60C 109.5 . . ? C601 C607 H60D 109.5 . . ? H60C C607 H60D 109.5 . . ? C601 C607 H60E 109.5 . . ? H60C C607 H60E 109.5 . . ? H60D C607 H60E 109.5 . . ? C603 C608 H60F 109.5 . . ? C603 C608 H60G 109.5 . . ? H60F C608 H60G 109.5 . . ? C603 C608 H60H 109.5 . . ? H60F C608 H60H 109.5 . . ? H60G C608 H60H 109.5 . . ? C605 C609 H60I 109.5 . . ? C605 C609 H60J 109.5 . . ? H60I C609 H60J 109.5 . . ? C605 C609 H60K 109.5 . . ? H60I C609 H60K 109.5 . . ? H60J C609 H60K 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si3 Ge1 Si1 C100 -62.94(15) . . . . ? Si2 Ge1 Si1 C100 -154.07(15) . . . . ? Ge2 Ge1 Si1 C100 -109.02(15) . . . . ? Si3 Ge1 Si1 C200 160.69(14) . . . . ? Si2 Ge1 Si1 C200 69.56(15) . . . . ? Ge2 Ge1 Si1 C200 114.61(15) . . . . ? Si3 Ge1 Si1 Ge2 46.08(3) . . . . ? Si2 Ge1 Si1 Ge2 -45.05(4) . . . . ? C100 Si1 Ge2 Si2 158.04(14) . . . . ? C200 Si1 Ge2 Si2 -64.29(15) . . . . ? Ge1 Si1 Ge2 Si2 45.40(4) . . . . ? C100 Si1 Ge2 Si3 67.55(14) . . . . ? C200 Si1 Ge2 Si3 -154.78(15) . . . . ? Ge1 Si1 Ge2 Si3 -45.09(3) . . . . ? C100 Si1 Ge2 Ge1 112.64(14) . . . . ? C200 Si1 Ge2 Ge1 -109.69(15) . . . . ? Si3 Ge1 Ge2 Si2 120.44(5) . . . . ? Si1 Ge1 Ge2 Si2 -120.10(5) . . . . ? Si3 Ge1 Ge2 Si1 -119.46(5) . . . . ? Si2 Ge1 Ge2 Si1 120.10(5) . . . . ? Si1 Ge1 Ge2 Si3 119.46(5) . . . . ? Si2 Ge1 Ge2 Si3 -120.44(5) . . . . ? Si1 Ge2 Si2 C400 -159.49(16) . . . . ? Si3 Ge2 Si2 C400 -69.79(16) . . . . ? Ge1 Ge2 Si2 C400 -114.32(16) . . . . ? Si1 Ge2 Si2 C300 63.00(16) . . . . ? Si3 Ge2 Si2 C300 152.70(15) . . . . ? Ge1 Ge2 Si2 C300 108.17(16) . . . . ? Si1 Ge2 Si2 Ge1 -45.17(4) . . . . ? Si3 Ge2 Si2 Ge1 44.53(3) . . . . ? Si3 Ge1 Si2 C400 63.44(15) . . . . ? Si1 Ge1 Si2 C400 154.21(15) . . . . ? Ge2 Ge1 Si2 C400 108.94(15) . . . . ? Si3 Ge1 Si2 C300 -158.61(15) . . . . ? Si1 Ge1 Si2 C300 -67.84(15) . . . . ? Ge2 Ge1 Si2 C300 -113.11(15) . . . . ? Si3 Ge1 Si2 Ge2 -45.50(4) . . . . ? Si1 Ge1 Si2 Ge2 45.27(4) . . . . ? Si1 Ge1 Si3 C500 -158.65(14) . . . . ? Si2 Ge1 Si3 C500 -68.14(14) . . . . ? Ge2 Ge1 Si3 C500 -113.00(14) . . . . ? Si1 Ge1 Si3 C600 64.66(14) . . . . ? Si2 Ge1 Si3 C600 155.17(14) . . . . ? Ge2 Ge1 Si3 C600 110.31(14) . . . . ? Si1 Ge1 Si3 Ge2 -45.65(3) . . . . ? Si2 Ge1 Si3 Ge2 44.86(4) . . . . ? Si2 Ge2 Si3 C500 63.54(14) . . . . ? Si1 Ge2 Si3 C500 154.28(14) . . . . ? Ge1 Ge2 Si3 C500 108.74(14) . . . . ? Si2 Ge2 Si3 C600 -158.78(15) . . . . ? Si1 Ge2 Si3 C600 -68.04(15) . . . . ? Ge1 Ge2 Si3 C600 -113.58(15) . . . . ? Si2 Ge2 Si3 Ge1 -45.20(4) . . . . ? Si1 Ge2 Si3 Ge1 45.54(3) . . . . ? C200 Si1 C100 C105 -115.8(3) . . . . ? Ge1 Si1 C100 C105 105.5(3) . . . . ? Ge2 Si1 C100 C105 25.7(4) . . . . ? C200 Si1 C100 C101 65.4(4) . . . . ? Ge1 Si1 C100 C101 -73.3(3) . . . . ? Ge2 Si1 C100 C101 -153.1(3) . . . . ? C105 C100 C101 C102 -2.5(6) . . . . ? Si1 C100 C101 C102 176.5(3) . . . . ? C105 C100 C101 C106 179.7(4) . . . . ? Si1 C100 C101 C106 -1.4(5) . . . . ? C100 C101 C102 C103 0.2(7) . . . . ? C106 C101 C102 C103 178.1(4) . . . . ? C101 C102 C103 C104 1.7(7) . . . . ? C101 C102 C103 C107 -176.5(5) . . . . ? C102 C103 C104 C105 -1.3(7) . . . . ? C107 C103 C104 C105 176.9(4) . . . . ? C103 C104 C105 C100 -1.0(7) . . . . ? C103 C104 C105 C108 179.2(4) . . . . ? C101 C100 C105 C104 2.9(6) . . . . ? Si1 C100 C105 C104 -176.0(3) . . . . ? C101 C100 C105 C108 -177.4(4) . . . . ? Si1 C100 C105 C108 3.8(6) . . . . ? C100 Si1 C200 C205 63.5(4) . . . . ? Ge1 Si1 C200 C205 -157.0(3) . . . . ? Ge2 Si1 C200 C205 -76.0(3) . . . . ? C100 Si1 C200 C201 -115.6(3) . . . . ? Ge1 Si1 C200 C201 23.9(4) . . . . ? Ge2 Si1 C200 C201 104.9(3) . . . . ? C205 C200 C201 C202 1.9(6) . . . . ? Si1 C200 C201 C202 -179.0(3) . . . . ? C205 C200 C201 C206 -178.8(4) . . . . ? Si1 C200 C201 C206 0.4(6) . . . . ? C200 C201 C202 C203 -1.1(6) . . . . ? C206 C201 C202 C203 179.6(4) . . . . ? C201 C202 C203 C204 0.0(7) . . . . ? C201 C202 C203 C207 178.4(4) . . . . ? C202 C203 C204 C205 0.2(7) . . . . ? C207 C203 C204 C205 -178.3(4) . . . . ? C203 C204 C205 C200 0.8(7) . . . . ? C203 C204 C205 C208 179.4(4) . . . . ? C201 C200 C205 C204 -1.8(6) . . . . ? Si1 C200 C205 C204 179.0(3) . . . . ? C201 C200 C205 C208 179.6(4) . . . . ? Si1 C200 C205 C208 0.4(5) . . . . ? C400 Si2 C300 C305 -118.7(4) . . . . ? Ge2 Si2 C300 C305 20.4(4) . . . . ? Ge1 Si2 C300 C305 100.0(4) . . . . ? C400 Si2 C300 C301 65.8(4) . . . . ? Ge2 Si2 C300 C301 -155.1(3) . . . . ? Ge1 Si2 C300 C301 -75.5(3) . . . . ? C305 C300 C301 C302 -3.0(6) . . . . ? Si2 C300 C301 C302 172.9(3) . . . . ? C305 C300 C301 C306 178.0(4) . . . . ? Si2 C300 C301 C306 -6.1(6) . . . . ? C300 C301 C302 C303 -0.1(7) . . . . ? C306 C301 C302 C303 178.9(4) . . . . ? C301 C302 C303 C304 3.2(7) . . . . ? C301 C302 C303 C307 -175.8(5) . . . . ? C302 C303 C304 C305 -3.1(7) . . . . ? C307 C303 C304 C305 175.9(5) . . . . ? C303 C304 C305 C300 0.0(7) . . . . ? C303 C304 C305 C308 179.5(4) . . . . ? C301 C300 C305 C304 3.0(6) . . . . ? Si2 C300 C305 C304 -172.5(3) . . . . ? C301 C300 C305 C308 -176.4(4) . . . . ? Si2 C300 C305 C308 8.0(6) . . . . ? C300 Si2 C400 C405 71.1(4) . . . . ? Ge2 Si2 C400 C405 -69.2(3) . . . . ? Ge1 Si2 C400 C405 -149.7(3) . . . . ? C300 Si2 C400 C401 -113.3(4) . . . . ? Ge2 Si2 C400 C401 106.3(3) . . . . ? Ge1 Si2 C400 C401 25.8(4) . . . . ? C405 C400 C401 C402 1.2(6) . . . . ? Si2 C400 C401 C402 -174.4(3) . . . . ? C405 C400 C401 C406 -178.2(4) . . . . ? Si2 C400 C401 C406 6.2(6) . . . . ? C400 C401 C402 C403 1.6(7) . . . . ? C406 C401 C402 C403 -178.9(4) . . . . ? C401 C402 C403 C404 -3.5(7) . . . . ? C401 C402 C403 C407 175.0(4) . . . . ? C402 C403 C404 C405 2.6(7) . . . . ? C407 C403 C404 C405 -175.9(5) . . . . ? C403 C404 C405 C400 0.1(7) . . . . ? C403 C404 C405 C408 -180.0(4) . . . . ? C401 C400 C405 C404 -2.0(6) . . . . ? Si2 C400 C405 C404 173.9(3) . . . . ? C401 C400 C405 C408 178.1(4) . . . . ? Si2 C400 C405 C408 -6.0(6) . . . . ? C600 Si3 C500 C505 -111.5(3) . . . . ? Ge1 Si3 C500 C505 108.4(3) . . . . ? Ge2 Si3 C500 C505 28.5(4) . . . . ? C600 Si3 C500 C501 70.9(3) . . . . ? Ge1 Si3 C500 C501 -69.3(3) . . . . ? Ge2 Si3 C500 C501 -149.2(3) . . . . ? C505 C500 C501 C502 -2.2(6) . . . . ? Si3 C500 C501 C502 175.7(3) . . . . ? C505 C500 C501 C506 179.7(4) . . . . ? Si3 C500 C501 C506 -2.4(5) . . . . ? C500 C501 C502 C503 0.1(6) . . . . ? C506 C501 C502 C503 178.4(4) . . . . ? C501 C502 C503 C504 2.9(6) . . . . ? C501 C502 C503 C507 -176.4(4) . . . . ? C502 C503 C504 C505 -4.1(6) . . . . ? C507 C503 C504 C505 175.3(4) . . . . ? C503 C504 C505 C500 2.1(6) . . . . ? C503 C504 C505 C508 -177.9(4) . . . . ? C501 C500 C505 C504 1.1(6) . . . . ? Si3 C500 C505 C504 -176.6(3) . . . . ? C501 C500 C505 C508 -178.9(4) . . . . ? Si3 C500 C505 C508 3.4(6) . . . . ? C500 Si3 C600 C605 63.8(3) . . . . ? Ge1 Si3 C600 C605 -157.8(3) . . . . ? Ge2 Si3 C600 C605 -76.9(3) . . . . ? C500 Si3 C600 C601 -117.2(3) . . . . ? Ge1 Si3 C600 C601 21.2(4) . . . . ? Ge2 Si3 C600 C601 102.0(3) . . . . ? C605 C600 C601 C602 3.3(6) . . . . ? Si3 C600 C601 C602 -175.6(3) . . . . ? C605 C600 C601 C607 -174.2(4) . . . . ? Si3 C600 C601 C607 6.8(6) . . . . ? C600 C601 C602 C603 -2.4(6) . . . . ? C607 C601 C602 C603 175.3(4) . . . . ? C601 C602 C603 C604 -0.8(7) . . . . ? C601 C602 C603 C608 179.7(5) . . . . ? C602 C603 C604 C605 3.2(7) . . . . ? C608 C603 C604 C605 -177.3(5) . . . . ? C603 C604 C605 C600 -2.2(7) . . . . ? C603 C604 C605 C609 178.4(4) . . . . ? C601 C600 C605 C604 -1.1(6) . . . . ? Si3 C600 C605 C604 177.9(3) . . . . ? C601 C600 C605 C609 178.3(4) . . . . ? Si3 C600 C605 C609 -2.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.734 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.084 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_2 _chemical_name_systematic ; Sn2Si3Mes6 ; _publ_section_exptl_refinement ; ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H66 Si3 Sn2' _chemical_formula_sum 'C54 H66 Si3 Sn2' _chemical_formula_weight 1036.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.5510(17) _cell_length_b 27.169(5) _cell_length_c 42.266(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9819(3) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 63751 _cell_measurement_theta_min 3.80 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63751 _diffrn_reflns_av_R_equivalents 0.1765 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8561 _reflns_number_gt 6822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+126.5737P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8561 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.25308(7) 0.36138(3) 0.373401(14) 0.02739(18) Uani 1 1 d . . . Si1 Si 0.3095(3) 0.44383(10) 0.40403(6) 0.0314(6) Uani 1 1 d . . . Sn2 Sn 0.57929(7) 0.39960(2) 0.393671(14) 0.02763(18) Uani 1 1 d . . . Si2 Si 0.4562(3) 0.31622(10) 0.41097(6) 0.0254(6) Uani 1 1 d . . . Si3 Si 0.4893(3) 0.38231(10) 0.33531(6) 0.0287(6) Uani 1 1 d . . . C100 C 0.4106(10) 0.3122(3) 0.4549(2) 0.0234(19) Uani 1 1 d . . . C101 C 0.2594(11) 0.3128(3) 0.4683(2) 0.025(2) Uani 1 1 d . . . C102 C 0.2431(11) 0.3123(4) 0.5007(2) 0.031(2) Uani 1 1 d . . . H10A H 0.1407 0.3116 0.5095 0.037 Uiso 1 1 calc R . . C103 C 0.3678(12) 0.3129(4) 0.5209(2) 0.033(2) Uani 1 1 d . . . C104 C 0.5165(12) 0.3112(4) 0.5083(2) 0.033(2) Uani 1 1 d . . . H10B H 0.6039 0.3104 0.5221 0.039 Uiso 1 1 calc R . . C105 C 0.5412(11) 0.3107(3) 0.4757(2) 0.027(2) Uani 1 1 d . . . C106 C 0.1097(11) 0.3149(4) 0.4493(2) 0.035(2) Uani 1 1 d . . . H10C H 0.0303 0.2942 0.4595 0.053 Uiso 1 1 calc R . . H10D H 0.1292 0.3027 0.4279 0.053 Uiso 1 1 calc R . . H10E H 0.0724 0.3489 0.4484 0.053 Uiso 1 1 calc R . . C107 C 0.3446(15) 0.3155(5) 0.5564(2) 0.051(3) Uani 1 1 d . . . H10F H 0.2327 0.3137 0.5613 0.077 Uiso 1 1 calc R . . H10G H 0.3873 0.3466 0.5644 0.077 Uiso 1 1 calc R . . H10H H 0.3989 0.2879 0.5665 0.077 Uiso 1 1 calc R . . C108 C 0.7088(11) 0.3097(4) 0.4644(2) 0.034(2) Uani 1 1 d . . . H10I H 0.7765 0.2978 0.4815 0.051 Uiso 1 1 calc R . . H10J H 0.7410 0.3430 0.4583 0.051 Uiso 1 1 calc R . . H10K H 0.7175 0.2877 0.4461 0.051 Uiso 1 1 calc R . . C200 C 0.5437(10) 0.2567(3) 0.3951(2) 0.0242(19) Uani 1 1 d . . . C201 C 0.4483(11) 0.2145(4) 0.3968(2) 0.030(2) Uani 1 1 d . . . C202 C 0.5025(13) 0.1696(4) 0.3845(2) 0.044(3) Uani 1 1 d . . . H20A H 0.4389 0.1412 0.3866 0.053 Uiso 1 1 calc R . . C203 C 0.6440(13) 0.1655(4) 0.3695(2) 0.043(3) Uani 1 1 d . . . C204 C 0.7355(11) 0.2068(4) 0.3687(2) 0.032(2) Uani 1 1 d . . . H20B H 0.8347 0.2044 0.3587 0.039 Uiso 1 1 calc R . . C205 C 0.6943(12) 0.2518(4) 0.3814(2) 0.034(2) Uani 1 1 d . . . C206 C 0.2876(12) 0.2149(4) 0.4112(3) 0.048(3) Uani 1 1 d . . . H20C H 0.2457 0.1813 0.4115 0.073 Uiso 1 1 calc R . . H20D H 0.2187 0.2360 0.3985 0.073 Uiso 1 1 calc R . . H20E H 0.2934 0.2276 0.4328 0.073 Uiso 1 1 calc R . . C207 C 0.6974(15) 0.1174(5) 0.3555(3) 0.065(4) Uani 1 1 d . . . H20F H 0.8114 0.1149 0.3572 0.098 Uiso 1 1 calc R . . H20G H 0.6669 0.1160 0.3331 0.098 Uiso 1 1 calc R . . H20H H 0.6487 0.0901 0.3670 0.098 Uiso 1 1 calc R . . C208 C 0.8115(11) 0.2920(4) 0.3806(2) 0.036(2) Uani 1 1 d . . . H20I H 0.8955 0.2834 0.3659 0.054 Uiso 1 1 calc R . . H20J H 0.8553 0.2967 0.4019 0.054 Uiso 1 1 calc R . . H20K H 0.7611 0.3225 0.3737 0.054 Uiso 1 1 calc R . . C300 C 0.5844(11) 0.3274(4) 0.3146(2) 0.030(2) Uani 1 1 d . . . C301 C 0.5122(12) 0.2825(4) 0.3087(2) 0.031(2) Uani 1 1 d . . . C302 C 0.5966(14) 0.2446(4) 0.2954(2) 0.042(3) Uani 1 1 d . . . H30A H 0.5459 0.2139 0.2920 0.050 Uiso 1 1 calc R . . C303 C 0.7531(14) 0.2493(4) 0.2867(2) 0.043(3) Uani 1 1 d . . . C304 C 0.8222(14) 0.2935(4) 0.2915(2) 0.045(3) Uani 1 1 d . . . H30B H 0.9284 0.2976 0.2854 0.054 Uiso 1 1 calc R . . C305 C 0.7434(12) 0.3330(4) 0.3050(2) 0.033(2) Uani 1 1 d . . . C306 C 0.3421(13) 0.2709(4) 0.3161(2) 0.041(3) Uani 1 1 d . . . H30C H 0.3097 0.2416 0.3043 0.061 Uiso 1 1 calc R . . H30D H 0.2764 0.2989 0.3101 0.061 Uiso 1 1 calc R . . H30E H 0.3308 0.2646 0.3389 0.061 Uiso 1 1 calc R . . C307 C 0.8405(17) 0.2064(5) 0.2731(3) 0.067(4) Uani 1 1 d . . . H30F H 0.9526 0.2140 0.2727 0.101 Uiso 1 1 calc R . . H30G H 0.8037 0.2001 0.2515 0.101 Uiso 1 1 calc R . . H30H H 0.8225 0.1772 0.2862 0.101 Uiso 1 1 calc R . . C308 C 0.8342(11) 0.3796(4) 0.3108(2) 0.039(3) Uani 1 1 d . . . H30I H 0.9210 0.3817 0.2957 0.059 Uiso 1 1 calc R . . H30J H 0.8757 0.3794 0.3325 0.059 Uiso 1 1 calc R . . H30K H 0.7651 0.4081 0.3081 0.059 Uiso 1 1 calc R . . C400 C 0.4740(11) 0.4377(3) 0.3080(2) 0.027(2) Uani 1 1 d . . . C401 C 0.3726(12) 0.4331(4) 0.2809(2) 0.036(2) Uani 1 1 d . . . C402 C 0.3544(13) 0.4730(4) 0.2613(2) 0.042(3) Uani 1 1 d . . . H40A H 0.2863 0.4694 0.2436 0.050 Uiso 1 1 calc R . . C403 C 0.4263(13) 0.5171(4) 0.2652(3) 0.044(3) Uani 1 1 d . . . C404 C 0.5263(12) 0.5206(4) 0.2918(2) 0.035(2) Uani 1 1 d . . . H40B H 0.5796 0.5508 0.2954 0.042 Uiso 1 1 calc R . . C405 C 0.5497(11) 0.4823(4) 0.3126(2) 0.031(2) Uani 1 1 d . . . C406 C 0.2829(12) 0.3874(4) 0.2742(2) 0.040(3) Uani 1 1 d . . . H40C H 0.2097 0.3933 0.2568 0.060 Uiso 1 1 calc R . . H40D H 0.2246 0.3777 0.2932 0.060 Uiso 1 1 calc R . . H40E H 0.3554 0.3610 0.2683 0.060 Uiso 1 1 calc R . . C407 C 0.4080(15) 0.5596(4) 0.2434(3) 0.057(3) Uani 1 1 d . . . H40F H 0.3871 0.5476 0.2219 0.085 Uiso 1 1 calc R . . H40G H 0.5044 0.5791 0.2433 0.085 Uiso 1 1 calc R . . H40H H 0.3206 0.5801 0.2505 0.085 Uiso 1 1 calc R . . C408 C 0.6602(13) 0.4930(4) 0.3397(2) 0.039(3) Uani 1 1 d . . . H40I H 0.7287 0.5205 0.3340 0.059 Uiso 1 1 calc R . . H40J H 0.7238 0.4638 0.3441 0.059 Uiso 1 1 calc R . . H40K H 0.5997 0.5017 0.3586 0.059 Uiso 1 1 calc R . . C500 C 0.2889(12) 0.5050(3) 0.3821(2) 0.033(2) Uani 1 1 d . . . C501 C 0.2044(11) 0.5110(4) 0.3539(3) 0.037(2) Uani 1 1 d . . . C502 C 0.2130(13) 0.5558(4) 0.3385(3) 0.042(3) Uani 1 1 d . . . H50A H 0.1551 0.5595 0.3195 0.051 Uiso 1 1 calc R . . C503 C 0.2981(13) 0.5949(4) 0.3487(3) 0.046(3) Uani 1 1 d . . . C504 C 0.3755(12) 0.5893(4) 0.3771(3) 0.038(3) Uani 1 1 d . . . H50B H 0.4326 0.6164 0.3854 0.046 Uiso 1 1 calc R . . C505 C 0.3726(12) 0.5457(4) 0.3937(2) 0.038(2) Uani 1 1 d . . . C506 C 0.1042(12) 0.4723(4) 0.3387(3) 0.045(3) Uani 1 1 d . . . H50C H 0.0468 0.4867 0.3209 0.067 Uiso 1 1 calc R . . H50D H 0.0299 0.4594 0.3543 0.067 Uiso 1 1 calc R . . H50E H 0.1706 0.4454 0.3310 0.067 Uiso 1 1 calc R . . C507 C 0.3097(17) 0.6419(5) 0.3301(3) 0.063(4) Uani 1 1 d . . . H50F H 0.2412 0.6400 0.3116 0.095 Uiso 1 1 calc R . . H50G H 0.4180 0.6468 0.3232 0.095 Uiso 1 1 calc R . . H50H H 0.2773 0.6696 0.3435 0.095 Uiso 1 1 calc R . . C508 C 0.4626(14) 0.5436(4) 0.4249(3) 0.052(3) Uani 1 1 d . . . H50I H 0.4927 0.5770 0.4312 0.078 Uiso 1 1 calc R . . H50J H 0.5567 0.5235 0.4222 0.078 Uiso 1 1 calc R . . H50K H 0.3962 0.5290 0.4413 0.078 Uiso 1 1 calc R . . C600 C 0.2267(12) 0.4446(4) 0.4457(2) 0.034(2) Uani 1 1 d . . . C601 C 0.0620(14) 0.4481(4) 0.4479(3) 0.049(3) Uani 1 1 d . . . C602 C -0.0091(15) 0.4421(5) 0.4776(3) 0.060(4) Uani 1 1 d . . . H60A H -0.1199 0.4435 0.4790 0.072 Uiso 1 1 calc R . . C603 C 0.0766(18) 0.4343(4) 0.5049(3) 0.059(4) Uani 1 1 d . . . C604 C 0.2366(15) 0.4353(4) 0.5025(3) 0.049(3) Uani 1 1 d . . . H60B H 0.2965 0.4326 0.5214 0.059 Uiso 1 1 calc R . . C605 C 0.3156(14) 0.4401(4) 0.4739(2) 0.042(3) Uani 1 1 d . . . C606 C -0.0404(13) 0.4574(6) 0.4198(3) 0.071(4) Uani 1 1 d . . . H60C H -0.1481 0.4630 0.4269 0.107 Uiso 1 1 calc R . . H60D H -0.0375 0.4287 0.4057 0.107 Uiso 1 1 calc R . . H60E H -0.0026 0.4864 0.4084 0.107 Uiso 1 1 calc R . . C607 C -0.008(2) 0.4247(6) 0.5359(3) 0.098(6) Uani 1 1 d . . . H60F H 0.0649 0.4297 0.5536 0.148 Uiso 1 1 calc R . . H60G H -0.0461 0.3907 0.5363 0.148 Uiso 1 1 calc R . . H60H H -0.0960 0.4474 0.5380 0.148 Uiso 1 1 calc R . . C608 C 0.4928(13) 0.4389(4) 0.4751(2) 0.042(3) Uani 1 1 d . . . H60I H 0.5278 0.4418 0.4971 0.063 Uiso 1 1 calc R . . H60J H 0.5349 0.4664 0.4628 0.063 Uiso 1 1 calc R . . H60K H 0.5304 0.4078 0.4662 0.063 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 Sn1 0.0214(3) 0.0298(4) 0.0310(3) -0.0020(3) -0.0027(3) -0.0027(3) Si1 0.0265(14) 0.0282(15) 0.0396(15) -0.0054(12) -0.0061(12) 0.0018(12) Sn2 0.0221(3) 0.0308(4) 0.0300(3) -0.0022(3) -0.0020(3) -0.0031(3) Si2 0.0199(13) 0.0304(15) 0.0257(12) 0.0002(11) 0.0011(10) 0.0006(11) Si3 0.0261(13) 0.0343(15) 0.0258(13) -0.0011(11) -0.0030(11) -0.0040(12) C100 0.024(5) 0.021(5) 0.025(4) -0.003(4) 0.000(4) 0.000(4) C101 0.028(5) 0.014(5) 0.033(5) -0.003(4) 0.003(4) -0.004(4) C102 0.028(5) 0.032(6) 0.032(5) 0.002(4) 0.015(4) -0.008(4) C103 0.035(6) 0.032(6) 0.033(5) 0.000(4) 0.011(4) -0.004(5) C104 0.032(5) 0.037(6) 0.030(5) 0.001(4) -0.010(4) -0.004(5) C105 0.027(5) 0.029(6) 0.025(5) -0.002(4) -0.001(4) 0.001(4) C106 0.026(5) 0.037(6) 0.043(6) 0.001(5) -0.002(4) -0.001(5) C107 0.062(8) 0.053(8) 0.040(6) -0.002(5) 0.004(6) -0.011(7) C108 0.025(5) 0.037(6) 0.040(6) 0.004(5) -0.004(4) 0.004(5) C200 0.031(5) 0.020(5) 0.022(4) 0.002(4) 0.000(4) 0.002(4) C201 0.031(5) 0.034(6) 0.026(5) 0.000(4) 0.001(4) 0.001(4) C202 0.040(6) 0.047(7) 0.045(6) -0.004(5) -0.012(5) -0.002(6) C203 0.039(6) 0.044(7) 0.045(6) -0.017(5) -0.007(5) 0.012(6) C204 0.024(5) 0.045(7) 0.028(5) -0.008(4) 0.001(4) 0.013(5) C205 0.031(5) 0.046(7) 0.024(5) -0.001(4) -0.010(4) 0.006(5) C206 0.041(7) 0.042(7) 0.063(7) -0.016(6) 0.011(6) -0.017(5) C207 0.047(7) 0.055(8) 0.093(10) -0.030(7) -0.015(7) 0.015(7) C208 0.014(4) 0.059(7) 0.035(5) 0.002(5) 0.001(4) 0.006(5) C300 0.036(5) 0.032(6) 0.023(4) 0.008(4) -0.005(4) 0.005(5) C301 0.040(6) 0.035(6) 0.019(4) 0.004(4) -0.002(4) -0.001(5) C302 0.056(7) 0.038(6) 0.032(5) 0.000(5) -0.006(5) -0.001(6) C303 0.063(8) 0.036(7) 0.030(5) 0.002(5) 0.002(5) 0.011(6) C304 0.050(7) 0.057(8) 0.027(5) 0.001(5) 0.005(5) 0.007(6) C305 0.043(6) 0.027(6) 0.029(5) -0.001(4) -0.003(5) 0.002(5) C306 0.049(7) 0.036(6) 0.038(6) -0.001(5) -0.004(5) -0.013(5) C307 0.083(10) 0.065(9) 0.053(7) -0.006(7) 0.016(7) 0.021(8) C308 0.025(5) 0.053(7) 0.039(6) 0.002(5) 0.004(4) -0.009(5) C400 0.034(5) 0.025(5) 0.023(4) -0.001(4) 0.001(4) -0.006(4) C401 0.038(6) 0.040(6) 0.031(5) 0.002(5) 0.011(4) 0.003(5) C402 0.046(6) 0.048(7) 0.031(5) 0.008(5) -0.003(5) 0.002(6) C403 0.036(6) 0.049(7) 0.047(6) 0.009(5) 0.010(5) 0.001(6) C404 0.030(5) 0.036(6) 0.039(6) -0.002(5) 0.009(5) 0.002(5) C405 0.027(5) 0.032(6) 0.032(5) 0.005(4) 0.010(4) 0.003(4) C406 0.043(6) 0.042(6) 0.034(5) 0.005(5) -0.011(5) -0.009(5) C407 0.059(8) 0.048(7) 0.064(8) 0.017(6) -0.001(7) -0.002(7) C408 0.046(6) 0.036(6) 0.037(6) -0.002(5) -0.001(5) -0.009(5) C500 0.033(6) 0.020(5) 0.045(6) 0.000(4) 0.005(4) 0.003(4) C501 0.024(5) 0.037(6) 0.051(6) -0.004(5) -0.004(5) 0.005(5) C502 0.037(6) 0.042(7) 0.048(6) -0.005(5) 0.002(5) 0.009(5) C503 0.043(6) 0.053(8) 0.043(6) 0.003(6) 0.012(5) 0.020(6) C504 0.035(6) 0.021(5) 0.058(7) -0.013(5) 0.008(5) 0.001(4) C505 0.032(5) 0.038(6) 0.045(6) -0.012(5) 0.007(5) 0.007(5) C506 0.035(6) 0.052(7) 0.047(6) -0.003(5) -0.016(5) 0.006(5) C507 0.073(9) 0.044(8) 0.073(9) 0.021(7) -0.002(7) -0.004(7) C508 0.051(7) 0.041(7) 0.063(8) -0.008(6) -0.014(6) -0.009(6) C600 0.038(6) 0.024(5) 0.039(5) -0.010(4) 0.008(5) -0.003(5) C601 0.045(7) 0.038(7) 0.065(8) -0.023(6) 0.017(6) -0.008(6) C602 0.046(7) 0.048(8) 0.084(10) -0.018(7) 0.021(7) -0.003(6) C603 0.084(10) 0.026(6) 0.068(8) -0.010(6) 0.029(8) 0.002(7) C604 0.063(8) 0.038(7) 0.047(6) -0.009(5) 0.003(6) -0.003(6) C605 0.068(8) 0.027(6) 0.032(5) -0.010(4) 0.013(5) 0.000(6) C606 0.018(6) 0.101(12) 0.095(10) -0.047(9) 0.007(6) 0.015(7) C607 0.149(16) 0.074(11) 0.073(10) -0.002(8) 0.069(11) 0.006(11) C608 0.057(7) 0.034(6) 0.035(6) -0.008(5) -0.012(5) -0.004(6) _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 Sn1 Si1 2.632(3) . ? Sn1 Si3 2.645(3) . ? Sn1 Si2 2.654(3) . ? Sn1 Sn2 3.0973(10) . ? Si1 C600 1.899(10) . ? Si1 C500 1.912(10) . ? Si1 Sn2 2.637(3) . ? Sn2 Si2 2.603(3) . ? Sn2 Si3 2.626(3) . ? Si2 C100 1.898(9) . ? Si2 C200 1.905(9) . ? Si3 C400 1.900(10) . ? Si3 C300 1.910(10) . ? C100 C101 1.412(12) . ? C100 C105 1.423(12) . ? C101 C102 1.380(12) . ? C101 C106 1.511(13) . ? C102 C103 1.364(14) . ? C102 H10A 0.9500 . ? C103 C104 1.379(13) . ? C103 C107 1.516(13) . ? C104 C105 1.393(12) . ? C104 H10B 0.9500 . ? C105 C108 1.511(13) . ? C106 H10C 0.9800 . ? C106 H10D 0.9800 . ? C106 H10E 0.9800 . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? C107 H10H 0.9800 . ? C108 H10I 0.9800 . ? C108 H10J 0.9800 . ? C108 H10K 0.9800 . ? C200 C201 1.410(13) . ? C200 C205 1.417(13) . ? C201 C202 1.404(14) . ? C201 C206 1.502(13) . ? C202 C203 1.371(15) . ? C202 H20A 0.9500 . ? C203 C204 1.368(15) . ? C203 C207 1.506(15) . ? C204 C205 1.379(14) . ? C204 H20B 0.9500 . ? C205 C208 1.483(14) . ? C206 H20C 0.9800 . ? C206 H20D 0.9800 . ? C206 H20E 0.9800 . ? C207 H20F 0.9800 . ? C207 H20G 0.9800 . ? C207 H20H 0.9800 . ? C208 H20I 0.9800 . ? C208 H20J 0.9800 . ? C208 H20K 0.9800 . ? C300 C301 1.392(14) . ? C300 C305 1.427(14) . ? C301 C302 1.378(14) . ? C301 C306 1.521(14) . ? C302 C303 1.393(16) . ? C302 H30A 0.9500 . ? C303 C304 1.354(16) . ? C303 C307 1.498(15) . ? C304 C305 1.392(14) . ? C304 H30B 0.9500 . ? C305 C308 1.505(14) . ? C306 H30C 0.9800 . ? C306 H30D 0.9800 . ? C306 H30E 0.9800 . ? C307 H30F 0.9800 . ? C307 H30G 0.9800 . ? C307 H30H 0.9800 . ? C308 H30I 0.9800 . ? C308 H30J 0.9800 . ? C308 H30K 0.9800 . ? C400 C405 1.388(13) . ? C400 C401 1.444(13) . ? C401 C402 1.374(14) . ? C401 C406 1.486(14) . ? C402 C403 1.357(15) . ? C402 H40A 0.9500 . ? C403 C404 1.417(15) . ? C403 C407 1.486(15) . ? C404 C405 1.379(13) . ? C404 H40B 0.9500 . ? C405 C408 1.513(14) . ? C406 H40C 0.9800 . ? C406 H40D 0.9800 . ? C406 H40E 0.9800 . ? C407 H40F 0.9800 . ? C407 H40G 0.9800 . ? C407 H40H 0.9800 . ? C408 H40I 0.9800 . ? C408 H40J 0.9800 . ? C408 H40K 0.9800 . ? C500 C501 1.404(14) . ? C500 C505 1.405(14) . ? C501 C502 1.381(15) . ? C501 C506 1.500(14) . ? C502 C503 1.358(16) . ? C502 H50A 0.9500 . ? C503 C504 1.378(15) . ? C503 C507 1.502(15) . ? C504 C505 1.380(15) . ? C504 H50B 0.9500 . ? C505 C508 1.526(15) . ? C506 H50C 0.9800 . ? C506 H50D 0.9800 . ? C506 H50E 0.9800 . ? C507 H50F 0.9800 . ? C507 H50G 0.9800 . ? C507 H50H 0.9800 . ? C508 H50I 0.9800 . ? C508 H50J 0.9800 . ? C508 H50K 0.9800 . ? C600 C601 1.415(15) . ? C600 C605 1.420(15) . ? C601 C602 1.405(17) . ? C601 C606 1.498(17) . ? C602 C603 1.383(19) . ? C602 H60A 0.9500 . ? C603 C604 1.372(18) . ? C603 C607 1.519(17) . ? C604 C605 1.391(15) . ? C604 H60B 0.9500 . ? C605 C608 1.517(16) . ? C606 H60C 0.9800 . ? C606 H60D 0.9800 . ? C606 H60E 0.9800 . ? C607 H60F 0.9800 . ? C607 H60G 0.9800 . ? C607 H60H 0.9800 . ? C608 H60I 0.9800 . ? C608 H60J 0.9800 . ? C608 H60K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 Sn1 Si3 88.64(9) . . ? Si1 Sn1 Si2 88.80(8) . . ? Si3 Sn1 Si2 87.92(8) . . ? Si1 Sn1 Sn2 54.08(6) . . ? Si3 Sn1 Sn2 53.73(6) . . ? Si2 Sn1 Sn2 53.14(6) . . ? C600 Si1 C500 113.9(4) . . ? C600 Si1 Sn1 113.4(3) . . ? C500 Si1 Sn1 119.0(3) . . ? C600 Si1 Sn2 119.0(3) . . ? C500 Si1 Sn2 113.4(3) . . ? Sn1 Si1 Sn2 72.00(7) . . ? Si2 Sn2 Si3 89.41(8) . . ? Si2 Sn2 Si1 89.77(9) . . ? Si3 Sn2 Si1 88.93(9) . . ? Si2 Sn2 Sn1 54.66(6) . . ? Si3 Sn2 Sn1 54.30(6) . . ? Si1 Sn2 Sn1 53.92(6) . . ? C100 Si2 C200 112.2(4) . . ? C100 Si2 Sn2 114.0(3) . . ? C200 Si2 Sn2 118.7(3) . . ? C100 Si2 Sn1 118.5(3) . . ? C200 Si2 Sn1 116.0(3) . . ? Sn2 Si2 Sn1 72.20(7) . . ? C400 Si3 C300 111.7(4) . . ? C400 Si3 Sn2 116.6(3) . . ? C300 Si3 Sn2 116.4(3) . . ? C400 Si3 Sn1 119.1(3) . . ? C300 Si3 Sn1 115.8(3) . . ? Sn2 Si3 Sn1 71.97(7) . . ? C101 C100 C105 118.0(8) . . ? C101 C100 Si2 125.4(7) . . ? C105 C100 Si2 116.5(6) . . ? C102 C101 C100 119.5(8) . . ? C102 C101 C106 116.2(8) . . ? C100 C101 C106 124.3(8) . . ? C103 C102 C101 122.8(9) . . ? C103 C102 H10A 118.6 . . ? C101 C102 H10A 118.6 . . ? C102 C103 C104 118.7(9) . . ? C102 C103 C107 121.1(9) . . ? C104 C103 C107 120.2(9) . . ? C103 C104 C105 121.4(9) . . ? C103 C104 H10B 119.3 . . ? C105 C104 H10B 119.3 . . ? C104 C105 C100 119.6(8) . . ? C104 C105 C108 117.2(8) . . ? C100 C105 C108 123.2(8) . . ? C101 C106 H10C 109.5 . . ? C101 C106 H10D 109.5 . . ? H10C C106 H10D 109.5 . . ? C101 C106 H10E 109.5 . . ? H10C C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C103 C107 H10F 109.5 . . ? C103 C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C103 C107 H10H 109.5 . . ? H10F C107 H10H 109.5 . . ? H10G C107 H10H 109.5 . . ? C105 C108 H10I 109.5 . . ? C105 C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? C105 C108 H10K 109.5 . . ? H10I C108 H10K 109.5 . . ? H10J C108 H10K 109.5 . . ? C201 C200 C205 118.1(8) . . ? C201 C200 Si2 116.4(7) . . ? C205 C200 Si2 125.5(7) . . ? C202 C201 C200 119.7(9) . . ? C202 C201 C206 117.3(9) . . ? C200 C201 C206 123.0(9) . . ? C203 C202 C201 122.3(11) . . ? C203 C202 H20A 118.9 . . ? C201 C202 H20A 118.9 . . ? C204 C203 C202 116.7(10) . . ? C204 C203 C207 121.9(10) . . ? C202 C203 C207 121.3(11) . . ? C203 C204 C205 124.8(9) . . ? C203 C204 H20B 117.6 . . ? C205 C204 H20B 117.6 . . ? C204 C205 C200 118.3(10) . . ? C204 C205 C208 118.1(9) . . ? C200 C205 C208 123.6(9) . . ? C201 C206 H20C 109.5 . . ? C201 C206 H20D 109.5 . . ? H20C C206 H20D 109.5 . . ? C201 C206 H20E 109.5 . . ? H20C C206 H20E 109.5 . . ? H20D C206 H20E 109.5 . . ? C203 C207 H20F 109.5 . . ? C203 C207 H20G 109.5 . . ? H20F C207 H20G 109.5 . . ? C203 C207 H20H 109.5 . . ? H20F C207 H20H 109.5 . . ? H20G C207 H20H 109.5 . . ? C205 C208 H20I 109.5 . . ? C205 C208 H20J 109.5 . . ? H20I C208 H20J 109.5 . . ? C205 C208 H20K 109.5 . . ? H20I C208 H20K 109.5 . . ? H20J C208 H20K 109.5 . . ? C301 C300 C305 117.7(9) . . ? C301 C300 Si3 125.4(8) . . ? C305 C300 Si3 116.9(7) . . ? C302 C301 C300 119.8(10) . . ? C302 C301 C306 115.5(9) . . ? C300 C301 C306 124.7(9) . . ? C301 C302 C303 122.9(11) . . ? C301 C302 H30A 118.6 . . ? C303 C302 H30A 118.6 . . ? C304 C303 C302 117.5(11) . . ? C304 C303 C307 121.9(12) . . ? C302 C303 C307 120.6(11) . . ? C303 C304 C305 122.3(11) . . ? C303 C304 H30B 118.8 . . ? C305 C304 H30B 118.8 . . ? C304 C305 C300 119.7(10) . . ? C304 C305 C308 117.8(10) . . ? C300 C305 C308 122.3(9) . . ? C301 C306 H30C 109.5 . . ? C301 C306 H30D 109.5 . . ? H30C C306 H30D 109.5 . . ? C301 C306 H30E 109.5 . . ? H30C C306 H30E 109.5 . . ? H30D C306 H30E 109.5 . . ? C303 C307 H30F 109.5 . . ? C303 C307 H30G 109.5 . . ? H30F C307 H30G 109.5 . . ? C303 C307 H30H 109.5 . . ? H30F C307 H30H 109.5 . . ? H30G C307 H30H 109.5 . . ? C305 C308 H30I 109.5 . . ? C305 C308 H30J 109.5 . . ? H30I C308 H30J 109.5 . . ? C305 C308 H30K 109.5 . . ? H30I C308 H30K 109.5 . . ? H30J C308 H30K 109.5 . . ? C405 C400 C401 117.9(9) . . ? C405 C400 Si3 125.0(7) . . ? C401 C400 Si3 117.1(7) . . ? C402 C401 C400 118.7(10) . . ? C402 C401 C406 119.1(10) . . ? C400 C401 C406 122.1(9) . . ? C403 C402 C401 124.9(10) . . ? C403 C402 H40A 117.6 . . ? C401 C402 H40A 117.6 . . ? C402 C403 C404 115.5(10) . . ? C402 C403 C407 124.3(11) . . ? C404 C403 C407 120.2(11) . . ? C405 C404 C403 122.9(10) . . ? C405 C404 H40B 118.5 . . ? C403 C404 H40B 118.5 . . ? C404 C405 C400 120.1(9) . . ? C404 C405 C408 115.4(9) . . ? C400 C405 C408 124.4(9) . . ? C401 C406 H40C 109.5 . . ? C401 C406 H40D 109.5 . . ? H40C C406 H40D 109.5 . . ? C401 C406 H40E 109.5 . . ? H40C C406 H40E 109.5 . . ? H40D C406 H40E 109.5 . . ? C403 C407 H40F 109.5 . . ? C403 C407 H40G 109.5 . . ? H40F C407 H40G 109.5 . . ? C403 C407 H40H 109.5 . . ? H40F C407 H40H 109.5 . . ? H40G C407 H40H 109.5 . . ? C405 C408 H40I 109.5 . . ? C405 C408 H40J 109.5 . . ? H40I C408 H40J 109.5 . . ? C405 C408 H40K 109.5 . . ? H40I C408 H40K 109.5 . . ? H40J C408 H40K 109.5 . . ? C501 C500 C505 118.0(9) . . ? C501 C500 Si1 124.0(8) . . ? C505 C500 Si1 117.8(8) . . ? C502 C501 C500 118.2(10) . . ? C502 C501 C506 116.6(10) . . ? C500 C501 C506 125.3(10) . . ? C503 C502 C501 124.8(11) . . ? C503 C502 H50A 117.6 . . ? C501 C502 H50A 117.6 . . ? C502 C503 C504 116.6(11) . . ? C502 C503 C507 122.4(11) . . ? C504 C503 C507 121.0(12) . . ? C503 C504 C505 122.0(10) . . ? C503 C504 H50B 119.0 . . ? C505 C504 H50B 119.0 . . ? C504 C505 C500 120.4(10) . . ? C504 C505 C508 117.6(10) . . ? C500 C505 C508 122.0(10) . . ? C501 C506 H50C 109.5 . . ? C501 C506 H50D 109.5 . . ? H50C C506 H50D 109.5 . . ? C501 C506 H50E 109.5 . . ? H50C C506 H50E 109.5 . . ? H50D C506 H50E 109.5 . . ? C503 C507 H50F 109.5 . . ? C503 C507 H50G 109.5 . . ? H50F C507 H50G 109.5 . . ? C503 C507 H50H 109.5 . . ? H50F C507 H50H 109.5 . . ? H50G C507 H50H 109.5 . . ? C505 C508 H50I 109.5 . . ? C505 C508 H50J 109.5 . . ? H50I C508 H50J 109.5 . . ? C505 C508 H50K 109.5 . . ? H50I C508 H50K 109.5 . . ? H50J C508 H50K 109.5 . . ? C601 C600 C605 118.9(10) . . ? C601 C600 Si1 115.7(8) . . ? C605 C600 Si1 125.4(8) . . ? C602 C601 C600 118.8(12) . . ? C602 C601 C606 118.5(11) . . ? C600 C601 C606 122.7(10) . . ? C603 C602 C601 122.3(12) . . ? C603 C602 H60A 118.9 . . ? C601 C602 H60A 118.9 . . ? C604 C603 C602 117.7(12) . . ? C604 C603 C607 122.7(15) . . ? C602 C603 C607 119.7(14) . . ? C603 C604 C605 123.3(12) . . ? C603 C604 H60B 118.3 . . ? C605 C604 H60B 118.3 . . ? C604 C605 C600 118.6(11) . . ? C604 C605 C608 117.1(11) . . ? C600 C605 C608 124.3(9) . . ? C601 C606 H60C 109.5 . . ? C601 C606 H60D 109.5 . . ? H60C C606 H60D 109.5 . . ? C601 C606 H60E 109.5 . . ? H60C C606 H60E 109.5 . . ? H60D C606 H60E 109.5 . . ? C603 C607 H60F 109.5 . . ? C603 C607 H60G 109.5 . . ? H60F C607 H60G 109.5 . . ? C603 C607 H60H 109.5 . . ? H60F C607 H60H 109.5 . . ? H60G C607 H60H 109.5 . . ? C605 C608 H60I 109.5 . . ? C605 C608 H60J 109.5 . . ? H60I C608 H60J 109.5 . . ? C605 C608 H60K 109.5 . . ? H60I C608 H60K 109.5 . . ? H60J C608 H60K 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si3 Sn1 Si1 C600 -159.0(4) . . . . ? Si2 Sn1 Si1 C600 -71.1(4) . . . . ? Sn2 Sn1 Si1 C600 -114.6(4) . . . . ? Si3 Sn1 Si1 C500 62.8(4) . . . . ? Si2 Sn1 Si1 C500 150.7(4) . . . . ? Sn2 Sn1 Si1 C500 107.2(4) . . . . ? Si3 Sn1 Si1 Sn2 -44.48(7) . . . . ? Si2 Sn1 Si1 Sn2 43.47(7) . . . . ? C600 Si1 Sn2 Si2 62.8(4) . . . . ? C500 Si1 Sn2 Si2 -159.0(4) . . . . ? Sn1 Si1 Sn2 Si2 -44.53(7) . . . . ? C600 Si1 Sn2 Si3 152.2(4) . . . . ? C500 Si1 Sn2 Si3 -69.6(4) . . . . ? Sn1 Si1 Sn2 Si3 44.88(8) . . . . ? C600 Si1 Sn2 Sn1 107.3(4) . . . . ? C500 Si1 Sn2 Sn1 -114.5(4) . . . . ? Si1 Sn1 Sn2 Si2 120.71(10) . . . . ? Si3 Sn1 Sn2 Si2 -119.60(10) . . . . ? Si1 Sn1 Sn2 Si3 -119.69(11) . . . . ? Si2 Sn1 Sn2 Si3 119.60(10) . . . . ? Si3 Sn1 Sn2 Si1 119.69(11) . . . . ? Si2 Sn1 Sn2 Si1 -120.71(10) . . . . ? Si3 Sn2 Si2 C100 -158.8(3) . . . . ? Si1 Sn2 Si2 C100 -69.9(3) . . . . ? Sn1 Sn2 Si2 C100 -113.9(3) . . . . ? Si3 Sn2 Si2 C200 65.5(3) . . . . ? Si1 Sn2 Si2 C200 154.4(3) . . . . ? Sn1 Sn2 Si2 C200 110.4(3) . . . . ? Si3 Sn2 Si2 Sn1 -44.92(7) . . . . ? Si1 Sn2 Si2 Sn1 44.01(7) . . . . ? Si1 Sn1 Si2 C100 64.0(3) . . . . ? Si3 Sn1 Si2 C100 152.7(3) . . . . ? Sn2 Sn1 Si2 C100 108.2(3) . . . . ? Si1 Sn1 Si2 C200 -158.0(3) . . . . ? Si3 Sn1 Si2 C200 -69.3(3) . . . . ? Sn2 Sn1 Si2 C200 -113.9(3) . . . . ? Si1 Sn1 Si2 Sn2 -44.14(8) . . . . ? Si3 Sn1 Si2 Sn2 44.55(7) . . . . ? Si2 Sn2 Si3 C400 159.4(4) . . . . ? Si1 Sn2 Si3 C400 69.6(4) . . . . ? Sn1 Sn2 Si3 C400 114.2(4) . . . . ? Si2 Sn2 Si3 C300 -65.3(4) . . . . ? Si1 Sn2 Si3 C300 -155.1(4) . . . . ? Sn1 Sn2 Si3 C300 -110.5(4) . . . . ? Si2 Sn2 Si3 Sn1 45.18(7) . . . . ? Si1 Sn2 Si3 Sn1 -44.61(8) . . . . ? Si1 Sn1 Si3 C400 -66.3(3) . . . . ? Si2 Sn1 Si3 C400 -155.1(3) . . . . ? Sn2 Sn1 Si3 C400 -111.0(3) . . . . ? Si1 Sn1 Si3 C300 156.0(3) . . . . ? Si2 Sn1 Si3 C300 67.1(3) . . . . ? Sn2 Sn1 Si3 C300 111.3(3) . . . . ? Si1 Sn1 Si3 Sn2 44.73(8) . . . . ? Si2 Sn1 Si3 Sn2 -44.12(7) . . . . ? C200 Si2 C100 C101 -112.8(8) . . . . ? Sn2 Si2 C100 C101 108.7(8) . . . . ? Sn1 Si2 C100 C101 26.7(9) . . . . ? C200 Si2 C100 C105 70.1(8) . . . . ? Sn2 Si2 C100 C105 -68.5(7) . . . . ? Sn1 Si2 C100 C105 -150.5(6) . . . . ? C105 C100 C101 C102 0.6(13) . . . . ? Si2 C100 C101 C102 -176.5(7) . . . . ? C105 C100 C101 C106 179.4(9) . . . . ? Si2 C100 C101 C106 2.3(13) . . . . ? C100 C101 C102 C103 2.1(15) . . . . ? C106 C101 C102 C103 -176.7(9) . . . . ? C101 C102 C103 C104 -3.6(15) . . . . ? C101 C102 C103 C107 176.2(9) . . . . ? C102 C103 C104 C105 2.3(15) . . . . ? C107 C103 C104 C105 -177.5(10) . . . . ? C103 C104 C105 C100 0.4(15) . . . . ? C103 C104 C105 C108 179.0(9) . . . . ? C101 C100 C105 C104 -1.8(14) . . . . ? Si2 C100 C105 C104 175.6(7) . . . . ? C101 C100 C105 C108 179.6(9) . . . . ? Si2 C100 C105 C108 -3.0(13) . . . . ? C100 Si2 C200 C201 62.4(8) . . . . ? Sn2 Si2 C200 C201 -161.2(6) . . . . ? Sn1 Si2 C200 C201 -78.1(7) . . . . ? C100 Si2 C200 C205 -118.4(8) . . . . ? Sn2 Si2 C200 C205 18.0(9) . . . . ? Sn1 Si2 C200 C205 101.1(7) . . . . ? C205 C200 C201 C202 -1.6(13) . . . . ? Si2 C200 C201 C202 177.7(7) . . . . ? C205 C200 C201 C206 179.0(9) . . . . ? Si2 C200 C201 C206 -1.8(12) . . . . ? C200 C201 C202 C203 -2.6(15) . . . . ? C206 C201 C202 C203 176.8(10) . . . . ? C201 C202 C203 C204 3.9(15) . . . . ? C201 C202 C203 C207 -177.8(10) . . . . ? C202 C203 C204 C205 -1.0(15) . . . . ? C207 C203 C204 C205 -179.3(10) . . . . ? C203 C204 C205 C200 -3.1(14) . . . . ? C203 C204 C205 C208 175.7(9) . . . . ? C201 C200 C205 C204 4.2(13) . . . . ? Si2 C200 C205 C204 -174.9(7) . . . . ? C201 C200 C205 C208 -174.5(8) . . . . ? Si2 C200 C205 C208 6.4(13) . . . . ? C400 Si3 C300 C301 -116.8(8) . . . . ? Sn2 Si3 C300 C301 105.8(8) . . . . ? Sn1 Si3 C300 C301 24.0(9) . . . . ? C400 Si3 C300 C305 64.4(8) . . . . ? Sn2 Si3 C300 C305 -73.1(7) . . . . ? Sn1 Si3 C300 C305 -154.8(6) . . . . ? C305 C300 C301 C302 3.1(13) . . . . ? Si3 C300 C301 C302 -175.8(7) . . . . ? C305 C300 C301 C306 -177.5(9) . . . . ? Si3 C300 C301 C306 3.7(13) . . . . ? C300 C301 C302 C303 -1.5(15) . . . . ? C306 C301 C302 C303 179.0(9) . . . . ? C301 C302 C303 C304 -0.7(15) . . . . ? C301 C302 C303 C307 178.4(10) . . . . ? C302 C303 C304 C305 1.1(15) . . . . ? C307 C303 C304 C305 -178.0(10) . . . . ? C303 C304 C305 C300 0.6(15) . . . . ? C303 C304 C305 C308 176.8(9) . . . . ? C301 C300 C305 C304 -2.7(13) . . . . ? Si3 C300 C305 C304 176.2(7) . . . . ? C301 C300 C305 C308 -178.7(8) . . . . ? Si3 C300 C305 C308 0.2(12) . . . . ? C300 Si3 C400 C405 -116.1(8) . . . . ? Sn2 Si3 C400 C405 21.2(9) . . . . ? Sn1 Si3 C400 C405 104.5(8) . . . . ? C300 Si3 C400 C401 65.4(8) . . . . ? Sn2 Si3 C400 C401 -157.2(6) . . . . ? Sn1 Si3 C400 C401 -73.9(8) . . . . ? C405 C400 C401 C402 -0.8(14) . . . . ? Si3 C400 C401 C402 177.7(8) . . . . ? C405 C400 C401 C406 -178.4(9) . . . . ? Si3 C400 C401 C406 0.1(13) . . . . ? C400 C401 C402 C403 0.7(16) . . . . ? C406 C401 C402 C403 178.4(10) . . . . ? C401 C402 C403 C404 -0.2(16) . . . . ? C401 C402 C403 C407 178.7(11) . . . . ? C402 C403 C404 C405 -0.2(15) . . . . ? C407 C403 C404 C405 -179.1(10) . . . . ? C403 C404 C405 C400 0.1(15) . . . . ? C403 C404 C405 C408 -179.8(9) . . . . ? C401 C400 C405 C404 0.4(14) . . . . ? Si3 C400 C405 C404 -178.0(7) . . . . ? C401 C400 C405 C408 -179.7(9) . . . . ? Si3 C400 C405 C408 1.9(14) . . . . ? C600 Si1 C500 C501 -119.1(9) . . . . ? Sn1 Si1 C500 C501 18.9(10) . . . . ? Sn2 Si1 C500 C501 100.6(8) . . . . ? C600 Si1 C500 C505 65.6(9) . . . . ? Sn1 Si1 C500 C505 -156.4(6) . . . . ? Sn2 Si1 C500 C505 -74.7(8) . . . . ? C505 C500 C501 C502 2.4(14) . . . . ? Si1 C500 C501 C502 -172.9(8) . . . . ? C505 C500 C501 C506 -177.7(9) . . . . ? Si1 C500 C501 C506 7.1(15) . . . . ? C500 C501 C502 C503 0.3(16) . . . . ? C506 C501 C502 C503 -179.7(10) . . . . ? C501 C502 C503 C504 -2.8(16) . . . . ? C501 C502 C503 C507 176.7(11) . . . . ? C502 C503 C504 C505 2.7(15) . . . . ? C507 C503 C504 C505 -176.9(10) . . . . ? C503 C504 C505 C500 -0.1(15) . . . . ? C503 C504 C505 C508 179.9(10) . . . . ? C501 C500 C505 C504 -2.5(14) . . . . ? Si1 C500 C505 C504 173.1(8) . . . . ? C501 C500 C505 C508 177.5(10) . . . . ? Si1 C500 C505 C508 -6.9(13) . . . . ? C500 Si1 C600 C601 69.1(9) . . . . ? Sn1 Si1 C600 C601 -71.3(9) . . . . ? Sn2 Si1 C600 C601 -153.0(7) . . . . ? C500 Si1 C600 C605 -113.5(9) . . . . ? Sn1 Si1 C600 C605 106.1(9) . . . . ? Sn2 Si1 C600 C605 24.4(10) . . . . ? C605 C600 C601 C602 -6.3(16) . . . . ? Si1 C600 C601 C602 171.3(8) . . . . ? C605 C600 C601 C606 174.5(11) . . . . ? Si1 C600 C601 C606 -7.9(15) . . . . ? C600 C601 C602 C603 1.9(18) . . . . ? C606 C601 C602 C603 -178.9(12) . . . . ? C601 C602 C603 C604 3.7(19) . . . . ? C601 C602 C603 C607 -176.0(12) . . . . ? C602 C603 C604 C605 -5.0(19) . . . . ? C607 C603 C604 C605 174.7(11) . . . . ? C603 C604 C605 C600 0.6(18) . . . . ? C603 C604 C605 C608 -178.0(11) . . . . ? C601 C600 C605 C604 5.1(15) . . . . ? Si1 C600 C605 C604 -172.2(8) . . . . ? C601 C600 C605 C608 -176.4(10) . . . . ? Si1 C600 C605 C608 6.3(15) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.236 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.150 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_4 _chemical_name_systematic ; [FcS(Ge2Si3Mes6)SFc] ; _publ_section_exptl_refinement ; ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H84 Fe2 Ge2 S2 Si3, 2(C7 H8)' _chemical_formula_sum 'C88 H100 Fe2 Ge2 S2 Si3' _chemical_formula_weight 1562.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 23.038(5) _cell_length_b 15.932(3) _cell_length_c 21.740(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.82(3) _cell_angle_gamma 90.00 _cell_volume 7597(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 27778 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27778 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7427 _reflns_number_gt 5863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+17.7942P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7427 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1412 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _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 Ge1 Ge 0.555121(14) 0.34644(2) 0.231727(15) 0.02619(12) Uani 1 1 d . . . Fe1 Fe 0.76591(3) 0.28073(4) 0.19254(3) 0.05006(18) Uani 1 1 d . . . Si1 Si 0.54164(4) 0.28511(5) 0.32976(4) 0.0276(2) Uani 1 1 d . . . S1 S 0.63497(4) 0.36638(6) 0.19264(5) 0.0375(2) Uani 1 1 d . . . Si2 Si 0.5000 0.46912(7) 0.2500 0.0258(3) Uani 1 2 d S . . C10 C 0.68859(16) 0.2862(2) 0.21851(19) 0.0414(8) Uani 1 1 d . . . C11 C 0.74042(19) 0.2914(4) 0.2741(3) 0.0700(15) Uani 1 1 d . . . H11A H 0.7508 0.3382 0.3063 0.084 Uiso 1 1 calc R . . C12 C 0.7741(3) 0.2180(5) 0.2749(4) 0.109(3) Uani 1 1 d . . . H12A H 0.8137 0.2041 0.3082 0.131 Uiso 1 1 calc R . . C13 C 0.7453(3) 0.1683(3) 0.2246(5) 0.105(3) Uani 1 1 d . . . H13A H 0.7601 0.1124 0.2147 0.126 Uiso 1 1 calc R . . C14 C 0.6910(2) 0.2111(3) 0.1856(3) 0.0771(17) Uani 1 1 d . . . H14A H 0.6604 0.1901 0.1453 0.093 Uiso 1 1 calc R . . C20 C 0.7607(2) 0.3583(3) 0.1174(3) 0.0629(12) Uani 1 1 d . . . H20A H 0.7227 0.3842 0.0883 0.075 Uiso 1 1 calc R . . C21 C 0.7982(2) 0.3929(3) 0.1743(2) 0.0551(11) Uani 1 1 d . . . H21A H 0.7919 0.4480 0.1933 0.066 Uiso 1 1 calc R . . C22 C 0.8467(2) 0.3366(3) 0.2009(3) 0.0590(12) Uani 1 1 d . . . H22A H 0.8810 0.3448 0.2417 0.071 Uiso 1 1 calc R . . C23 C 0.8385(2) 0.2673(3) 0.1586(3) 0.0620(12) Uani 1 1 d . . . H23A H 0.8657 0.2170 0.1644 0.074 Uiso 1 1 calc R . . C24 C 0.7855(3) 0.2811(3) 0.1078(3) 0.0700(14) Uani 1 1 d . . . H24A H 0.7679 0.2421 0.0707 0.084 Uiso 1 1 calc R . . C100 C 0.54173(15) 0.1671(2) 0.34021(17) 0.0335(7) Uani 1 1 d . . . C101 C 0.51191(18) 0.1354(2) 0.38359(18) 0.0418(8) Uani 1 1 d . . . C102 C 0.5106(2) 0.0502(3) 0.3942(2) 0.0601(12) Uani 1 1 d . . . H10A H 0.4902 0.0303 0.4232 0.072 Uiso 1 1 calc R . . C103 C 0.5377(2) -0.0071(3) 0.3642(3) 0.0677(14) Uani 1 1 d . . . C104 C 0.5665(2) 0.0240(3) 0.3223(2) 0.0561(11) Uani 1 1 d . . . H10B H 0.5850 -0.0146 0.3007 0.067 Uiso 1 1 calc R . . C105 C 0.56993(16) 0.1086(2) 0.30996(19) 0.0401(8) Uani 1 1 d . . . C106 C 0.4802(2) 0.1912(3) 0.4185(2) 0.0474(9) Uani 1 1 d . . . H10C H 0.4584 0.1567 0.4416 0.071 Uiso 1 1 calc R . . H10D H 0.4511 0.2272 0.3873 0.071 Uiso 1 1 calc R . . H10E H 0.5103 0.2262 0.4495 0.071 Uiso 1 1 calc R . . C107 C 0.5343(3) -0.1006(3) 0.3752(4) 0.110(3) Uani 1 1 d . . . H10F H 0.5744 -0.1259 0.3809 0.166 Uiso 1 1 calc R . . H10G H 0.5043 -0.1261 0.3379 0.166 Uiso 1 1 calc R . . H10H H 0.5222 -0.1103 0.4141 0.166 Uiso 1 1 calc R . . C108 C 0.60394(17) 0.1319(2) 0.26377(19) 0.0408(8) Uani 1 1 d . . . H10I H 0.5883 0.0991 0.2240 0.061 Uiso 1 1 calc R . . H10J H 0.6474 0.1201 0.2835 0.061 Uiso 1 1 calc R . . H10K H 0.5983 0.1919 0.2536 0.061 Uiso 1 1 calc R . . C200 C 0.58801(15) 0.3339(2) 0.40925(16) 0.0310(7) Uani 1 1 d . . . C201 C 0.56468(16) 0.3831(2) 0.45010(16) 0.0347(7) Uani 1 1 d . . . C202 C 0.60358(18) 0.4119(2) 0.50831(17) 0.0405(8) Uani 1 1 d . . . H20B H 0.5870 0.4445 0.5355 0.049 Uiso 1 1 calc R . . C203 C 0.66527(18) 0.3954(2) 0.52843(17) 0.0425(9) Uani 1 1 d . . . C204 C 0.68831(17) 0.3476(2) 0.48820(18) 0.0427(9) Uani 1 1 d . . . H20C H 0.7309 0.3366 0.5006 0.051 Uiso 1 1 calc R . . C205 C 0.65141(16) 0.3155(2) 0.43056(16) 0.0367(8) Uani 1 1 d . . . C206 C 0.49920(16) 0.4082(2) 0.43393(17) 0.0378(8) Uani 1 1 d . . . H20D H 0.4896 0.4214 0.4738 0.057 Uiso 1 1 calc R . . H20E H 0.4733 0.3620 0.4115 0.057 Uiso 1 1 calc R . . H20F H 0.4918 0.4578 0.4059 0.057 Uiso 1 1 calc R . . C207 C 0.7066(2) 0.4287(3) 0.5912(2) 0.0600(12) Uani 1 1 d . . . H20G H 0.6838 0.4674 0.6103 0.090 Uiso 1 1 calc R . . H20H H 0.7409 0.4586 0.5833 0.090 Uiso 1 1 calc R . . H20I H 0.7222 0.3820 0.6210 0.090 Uiso 1 1 calc R . . C208 C 0.68050(17) 0.2630(3) 0.39100(18) 0.0448(9) Uani 1 1 d . . . H20J H 0.7250 0.2676 0.4085 0.067 Uiso 1 1 calc R . . H20K H 0.6672 0.2828 0.3462 0.067 Uiso 1 1 calc R . . H20L H 0.6683 0.2042 0.3924 0.067 Uiso 1 1 calc R . . C300 C 0.53655(14) 0.53815(19) 0.32270(15) 0.0283(6) Uani 1 1 d . . . C301 C 0.49810(15) 0.5921(2) 0.34424(16) 0.0323(7) Uani 1 1 d . . . C302 C 0.52117(17) 0.6440(2) 0.39685(17) 0.0367(8) Uani 1 1 d . . . H30A H 0.4943 0.6802 0.4098 0.044 Uiso 1 1 calc R . . C303 C 0.58266(17) 0.6444(2) 0.43120(16) 0.0367(8) Uani 1 1 d . . . C304 C 0.61991(16) 0.5921(2) 0.41018(16) 0.0356(7) Uani 1 1 d . . . H30B H 0.6622 0.5913 0.4334 0.043 Uiso 1 1 calc R . . C305 C 0.59912(15) 0.5404(2) 0.35687(15) 0.0308(7) Uani 1 1 d . . . C306 C 0.43026(16) 0.5949(2) 0.31195(18) 0.0415(8) Uani 1 1 d . . . H30C H 0.4114 0.6318 0.3365 0.062 Uiso 1 1 calc R . . H30D H 0.4134 0.5382 0.3105 0.062 Uiso 1 1 calc R . . H30E H 0.4218 0.6164 0.2679 0.062 Uiso 1 1 calc R . . C307 C 0.6074(2) 0.7007(3) 0.48850(19) 0.0530(10) Uani 1 1 d . . . H30F H 0.6470 0.7229 0.4885 0.079 Uiso 1 1 calc R . . H30G H 0.6122 0.6688 0.5283 0.079 Uiso 1 1 calc R . . H30H H 0.5790 0.7474 0.4862 0.079 Uiso 1 1 calc R . . C308 C 0.64641(15) 0.4913(2) 0.33758(17) 0.0361(8) Uani 1 1 d . . . H30I H 0.6851 0.4929 0.3727 0.054 Uiso 1 1 calc R . . H30J H 0.6521 0.5159 0.2985 0.054 Uiso 1 1 calc R . . H30K H 0.6329 0.4329 0.3290 0.054 Uiso 1 1 calc R . . C93 C 0.6551(4) 0.0082(5) 0.6022(4) 0.117(3) Uani 1 1 d . . . H93A H 0.6666 -0.0450 0.6219 0.140 Uiso 1 1 calc R . . C94 C 0.6324(6) 0.0689(6) 0.6320(4) 0.157(4) Uani 1 1 d . . . H94A H 0.6264 0.0561 0.6723 0.188 Uiso 1 1 calc R . . C95 C 0.6178(4) 0.1474(5) 0.6072(5) 0.122(3) Uani 1 1 d . . . H95A H 0.6020 0.1882 0.6297 0.147 Uiso 1 1 calc R . . C96 C 0.6256(3) 0.1649(6) 0.5534(4) 0.110(3) Uani 1 1 d . . . H96A H 0.6175 0.2202 0.5364 0.132 Uiso 1 1 calc R . . C97 C 0.6465(3) 0.1022(6) 0.5178(4) 0.108(3) Uani 1 1 d . . . H97A H 0.6500 0.1153 0.4765 0.130 Uiso 1 1 calc R . . C98 C 0.6610(3) 0.0259(6) 0.5423(4) 0.103(2) Uani 1 1 d . . . C99 C 0.6838(4) -0.0397(7) 0.5086(5) 0.171(5) Uani 1 1 d . . . H99A H 0.7203 -0.0195 0.4992 0.256 Uiso 1 1 calc R . . H99B H 0.6523 -0.0536 0.4681 0.256 Uiso 1 1 calc R . . H99C H 0.6938 -0.0898 0.5359 0.256 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 Ge1 0.02275(18) 0.02858(19) 0.0280(2) -0.00061(12) 0.00893(14) -0.00007(12) Fe1 0.0382(3) 0.0434(3) 0.0805(4) 0.0120(3) 0.0358(3) 0.0077(2) Si1 0.0255(4) 0.0296(4) 0.0276(4) 0.0027(3) 0.0082(3) 0.0032(3) S1 0.0310(4) 0.0406(5) 0.0466(5) 0.0024(4) 0.0203(4) 0.0014(3) Si2 0.0230(6) 0.0266(6) 0.0270(6) 0.000 0.0066(5) 0.000 C10 0.0284(17) 0.043(2) 0.057(2) 0.0100(17) 0.0206(17) 0.0049(15) C11 0.033(2) 0.115(4) 0.070(3) 0.034(3) 0.027(2) 0.012(2) C12 0.059(4) 0.118(6) 0.171(7) 0.099(6) 0.064(4) 0.040(4) C13 0.087(5) 0.039(3) 0.231(10) 0.041(4) 0.111(6) 0.019(3) C14 0.058(3) 0.043(2) 0.155(6) -0.006(3) 0.069(3) -0.004(2) C20 0.057(3) 0.061(3) 0.075(3) 0.017(2) 0.026(3) 0.000(2) C21 0.058(3) 0.041(2) 0.079(3) 0.006(2) 0.039(2) 0.0021(19) C22 0.040(2) 0.065(3) 0.081(3) 0.012(2) 0.031(2) -0.009(2) C23 0.054(3) 0.061(3) 0.088(3) 0.002(2) 0.047(3) 0.008(2) C24 0.079(4) 0.068(3) 0.077(3) -0.005(3) 0.045(3) -0.004(3) C100 0.0310(17) 0.0311(17) 0.0375(18) 0.0059(14) 0.0091(14) 0.0040(13) C101 0.047(2) 0.0394(19) 0.043(2) 0.0110(16) 0.0201(17) 0.0078(16) C102 0.070(3) 0.046(2) 0.079(3) 0.023(2) 0.044(3) 0.009(2) C103 0.078(3) 0.037(2) 0.103(4) 0.019(2) 0.050(3) 0.012(2) C104 0.058(3) 0.038(2) 0.083(3) 0.006(2) 0.038(2) 0.0095(19) C105 0.0349(18) 0.0330(18) 0.053(2) 0.0014(16) 0.0133(16) 0.0034(14) C106 0.057(2) 0.046(2) 0.048(2) 0.0081(18) 0.030(2) 0.0049(19) C107 0.136(6) 0.044(3) 0.194(8) 0.036(4) 0.114(6) 0.023(3) C108 0.041(2) 0.0370(19) 0.049(2) -0.0022(16) 0.0207(17) 0.0037(15) C200 0.0298(16) 0.0350(17) 0.0273(16) 0.0041(13) 0.0074(13) 0.0019(13) C201 0.0402(19) 0.0324(17) 0.0322(17) 0.0045(14) 0.0122(15) 0.0018(14) C202 0.051(2) 0.0376(19) 0.0320(18) -0.0016(14) 0.0116(16) -0.0005(16) C203 0.048(2) 0.043(2) 0.0309(18) 0.0017(15) 0.0040(16) -0.0060(17) C204 0.0328(19) 0.050(2) 0.038(2) 0.0043(16) -0.0003(16) -0.0015(16) C205 0.0318(18) 0.045(2) 0.0300(17) 0.0083(15) 0.0044(14) 0.0044(15) C206 0.042(2) 0.0396(19) 0.0356(18) 0.0004(15) 0.0173(15) 0.0069(15) C207 0.067(3) 0.060(3) 0.043(2) -0.009(2) 0.001(2) -0.008(2) C208 0.0305(18) 0.065(3) 0.0361(19) 0.0043(17) 0.0067(15) 0.0110(17) C300 0.0294(16) 0.0282(16) 0.0281(16) 0.0011(12) 0.0101(13) -0.0008(12) C301 0.0358(18) 0.0286(16) 0.0333(17) 0.0014(13) 0.0118(14) 0.0004(13) C302 0.042(2) 0.0323(18) 0.0393(19) -0.0040(14) 0.0172(16) 0.0000(14) C303 0.046(2) 0.0358(18) 0.0293(17) -0.0038(14) 0.0123(15) -0.0098(15) C304 0.0342(18) 0.0400(19) 0.0293(17) 0.0028(14) 0.0048(14) -0.0068(15) C305 0.0298(16) 0.0309(16) 0.0311(16) 0.0010(13) 0.0081(13) -0.0027(13) C306 0.0339(19) 0.045(2) 0.045(2) -0.0062(16) 0.0123(16) 0.0089(15) C307 0.061(3) 0.060(3) 0.040(2) -0.0165(19) 0.0176(19) -0.016(2) C308 0.0237(16) 0.0392(18) 0.0414(19) 0.0009(15) 0.0042(14) -0.0005(14) C93 0.165(8) 0.069(4) 0.103(6) 0.020(4) 0.022(5) -0.024(5) C94 0.269(13) 0.093(6) 0.093(6) 0.019(5) 0.035(7) -0.031(7) C95 0.142(8) 0.088(5) 0.124(7) 0.007(5) 0.022(6) -0.019(5) C96 0.064(4) 0.125(6) 0.118(6) 0.059(5) -0.005(4) -0.017(4) C97 0.066(4) 0.148(7) 0.106(5) 0.058(5) 0.019(4) 0.004(4) C98 0.055(3) 0.136(7) 0.107(5) 0.010(5) 0.005(3) -0.015(4) C99 0.102(6) 0.209(12) 0.207(11) -0.079(9) 0.054(7) 0.005(7) _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 Ge1 S1 2.2724(10) . ? Ge1 Si1 2.4263(11) 2_655 ? Ge1 Si2 2.4287(11) . ? Ge1 Si1 2.4491(10) . ? Ge1 Ge1 2.8838(9) 2_655 ? Fe1 C12 2.009(6) . ? Fe1 C14 2.019(5) . ? Fe1 C21 2.021(4) . ? Fe1 C22 2.022(4) . ? Fe1 C20 2.023(5) . ? Fe1 C24 2.027(5) . ? Fe1 C10 2.028(4) . ? Fe1 C13 2.030(5) . ? Fe1 C23 2.037(4) . ? Fe1 C11 2.039(5) . ? Si1 C100 1.894(3) . ? Si1 C200 1.898(3) . ? Si1 Ge1 2.4263(11) 2_655 ? S1 C10 1.746(4) . ? Si2 C300 1.898(3) . ? Si2 C300 1.898(3) 2_655 ? Si2 Ge1 2.4287(11) 2_655 ? C10 C14 1.403(6) . ? C10 C11 1.418(6) . ? C11 C12 1.401(9) . ? C11 H11A 1.0000 . ? C12 C13 1.348(11) . ? C12 H12A 1.0000 . ? C13 C14 1.450(9) . ? C13 H13A 1.0000 . ? C14 H14A 1.0000 . ? C20 C21 1.388(7) . ? C20 C24 1.399(7) . ? C20 H20A 1.0000 . ? C21 C22 1.411(6) . ? C21 H21A 1.0000 . ? C22 C23 1.413(7) . ? C22 H22A 1.0000 . ? C23 C24 1.392(7) . ? C23 H23A 1.0000 . ? C24 H24A 1.0000 . ? C100 C105 1.408(5) . ? C100 C101 1.418(5) . ? C101 C102 1.379(5) . ? C101 C106 1.497(5) . ? C102 C103 1.378(6) . ? C102 H10A 0.9500 . ? C103 C104 1.374(6) . ? C103 C107 1.515(6) . ? C104 C105 1.382(5) . ? C104 H10B 0.9500 . ? C105 C108 1.497(5) . ? C106 H10C 0.9800 . ? C106 H10D 0.9800 . ? C106 H10E 0.9800 . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? C107 H10H 0.9800 . ? C108 H10I 0.9800 . ? C108 H10J 0.9800 . ? C108 H10K 0.9800 . ? C200 C201 1.409(5) . ? C200 C205 1.421(5) . ? C201 C202 1.386(5) . ? C201 C206 1.495(5) . ? C202 C203 1.378(5) . ? C202 H20B 0.9500 . ? C203 C204 1.382(6) . ? C203 C207 1.502(5) . ? C204 C205 1.379(5) . ? C204 H20C 0.9500 . ? C205 C208 1.497(5) . ? C206 H20D 0.9800 . ? C206 H20E 0.9800 . ? C206 H20F 0.9800 . ? C207 H20G 0.9800 . ? C207 H20H 0.9800 . ? C207 H20I 0.9800 . ? C208 H20J 0.9800 . ? C208 H20K 0.9800 . ? C208 H20L 0.9800 . ? C300 C305 1.406(5) . ? C300 C301 1.413(4) . ? C301 C302 1.378(5) . ? C301 C306 1.505(5) . ? C302 C303 1.385(5) . ? C302 H30A 0.9500 . ? C303 C304 1.371(5) . ? C303 C307 1.499(5) . ? C304 C305 1.382(5) . ? C304 H30B 0.9500 . ? C305 C308 1.502(5) . ? C306 H30C 0.9800 . ? C306 H30D 0.9800 . ? C306 H30E 0.9800 . ? C307 H30F 0.9800 . ? C307 H30G 0.9800 . ? C307 H30H 0.9800 . ? C308 H30I 0.9800 . ? C308 H30J 0.9800 . ? C308 H30K 0.9800 . ? C93 C94 1.357(12) . ? C93 C98 1.379(10) . ? C93 H93A 0.9500 . ? C94 C95 1.363(11) . ? C94 H94A 0.9500 . ? C95 C96 1.268(11) . ? C95 H95A 0.9500 . ? C96 C97 1.434(11) . ? C96 H96A 0.9500 . ? C97 C98 1.329(10) . ? C97 H97A 0.9500 . ? C98 C99 1.461(11) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ge1 Si1 124.24(4) . 2_655 ? S1 Ge1 Si2 118.18(3) . . ? Si1 Ge1 Si2 88.62(3) 2_655 . ? S1 Ge1 Si1 135.56(4) . . ? Si1 Ge1 Si1 88.80(4) 2_655 . ? Si2 Ge1 Si1 88.10(3) . . ? S1 Ge1 Ge1 170.06(3) . 2_655 ? Si1 Ge1 Ge1 54.10(3) 2_655 2_655 ? Si2 Ge1 Ge1 53.58(2) . 2_655 ? Si1 Ge1 Ge1 53.37(3) . 2_655 ? C12 Fe1 C14 68.8(3) . . ? C12 Fe1 C21 132.5(3) . . ? C14 Fe1 C21 146.0(2) . . ? C12 Fe1 C22 107.9(3) . . ? C14 Fe1 C22 172.77(19) . . ? C21 Fe1 C22 40.85(18) . . ? C12 Fe1 C20 172.0(3) . . ? C14 Fe1 C20 116.0(2) . . ? C21 Fe1 C20 40.2(2) . . ? C22 Fe1 C20 68.2(2) . . ? C12 Fe1 C24 145.6(3) . . ? C14 Fe1 C24 110.9(3) . . ? C21 Fe1 C24 67.8(2) . . ? C22 Fe1 C24 68.0(2) . . ? C20 Fe1 C24 40.4(2) . . ? C12 Fe1 C10 67.93(19) . . ? C14 Fe1 C10 40.58(17) . . ? C21 Fe1 C10 115.11(16) . . ? C22 Fe1 C10 145.03(19) . . ? C20 Fe1 C10 111.03(18) . . ? C24 Fe1 C10 135.4(2) . . ? C12 Fe1 C13 39.0(3) . . ? C14 Fe1 C13 42.0(3) . . ? C21 Fe1 C13 170.4(3) . . ? C22 Fe1 C13 131.5(3) . . ? C20 Fe1 C13 148.7(3) . . ? C24 Fe1 C13 117.1(3) . . ? C10 Fe1 C13 67.99(18) . . ? C12 Fe1 C23 114.0(2) . . ? C14 Fe1 C23 133.9(2) . . ? C21 Fe1 C23 68.22(18) . . ? C22 Fe1 C23 40.7(2) . . ? C20 Fe1 C23 67.9(2) . . ? C24 Fe1 C23 40.0(2) . . ? C10 Fe1 C23 173.91(19) . . ? C13 Fe1 C23 109.6(2) . . ? C12 Fe1 C11 40.5(3) . . ? C14 Fe1 C11 69.1(2) . . ? C21 Fe1 C11 108.5(2) . . ? C22 Fe1 C11 112.8(2) . . ? C20 Fe1 C11 133.6(2) . . ? C24 Fe1 C11 173.8(2) . . ? C10 Fe1 C11 40.81(17) . . ? C13 Fe1 C11 67.4(3) . . ? C23 Fe1 C11 144.3(2) . . ? C100 Si1 C200 108.52(15) . . ? C100 Si1 Ge1 115.66(11) . 2_655 ? C200 Si1 Ge1 120.21(11) . 2_655 ? C100 Si1 Ge1 120.31(12) . . ? C200 Si1 Ge1 116.30(11) . . ? Ge1 Si1 Ge1 72.52(3) 2_655 . ? C10 S1 Ge1 110.55(12) . . ? C300 Si2 C300 109.18(19) . 2_655 ? C300 Si2 Ge1 116.81(9) . 2_655 ? C300 Si2 Ge1 118.79(10) 2_655 2_655 ? C300 Si2 Ge1 118.79(10) . . ? C300 Si2 Ge1 116.81(9) 2_655 . ? Ge1 Si2 Ge1 72.84(4) 2_655 . ? C14 C10 C11 109.3(4) . . ? C14 C10 S1 126.4(4) . . ? C11 C10 S1 124.0(4) . . ? C14 C10 Fe1 69.3(2) . . ? C11 C10 Fe1 70.0(2) . . ? S1 C10 Fe1 122.5(2) . . ? C12 C11 C10 106.3(6) . . ? C12 C11 Fe1 68.6(4) . . ? C10 C11 Fe1 69.2(3) . . ? C12 C11 H11A 126.9 . . ? C10 C11 H11A 126.9 . . ? Fe1 C11 H11A 126.9 . . ? C13 C12 C11 110.3(6) . . ? C13 C12 Fe1 71.3(4) . . ? C11 C12 Fe1 70.9(3) . . ? C13 C12 H12A 124.8 . . ? C11 C12 H12A 124.8 . . ? Fe1 C12 H12A 124.8 . . ? C12 C13 C14 108.7(5) . . ? C12 C13 Fe1 69.7(3) . . ? C14 C13 Fe1 68.6(3) . . ? C12 C13 H13A 125.6 . . ? C14 C13 H13A 125.6 . . ? Fe1 C13 H13A 125.6 . . ? C10 C14 C13 105.4(6) . . ? C10 C14 Fe1 70.1(2) . . ? C13 C14 Fe1 69.4(3) . . ? C10 C14 H14A 127.3 . . ? C13 C14 H14A 127.3 . . ? Fe1 C14 H14A 127.3 . . ? C21 C20 C24 108.1(5) . . ? C21 C20 Fe1 69.8(3) . . ? C24 C20 Fe1 70.0(3) . . ? C21 C20 H20A 125.9 . . ? C24 C20 H20A 125.9 . . ? Fe1 C20 H20A 125.9 . . ? C20 C21 C22 108.2(4) . . ? C20 C21 Fe1 70.0(3) . . ? C22 C21 Fe1 69.6(2) . . ? C20 C21 H21A 125.9 . . ? C22 C21 H21A 125.9 . . ? Fe1 C21 H21A 125.9 . . ? C21 C22 C23 107.4(5) . . ? C21 C22 Fe1 69.5(2) . . ? C23 C22 Fe1 70.2(3) . . ? C21 C22 H22A 126.3 . . ? C23 C22 H22A 126.3 . . ? Fe1 C22 H22A 126.3 . . ? C24 C23 C22 107.6(4) . . ? C24 C23 Fe1 69.6(3) . . ? C22 C23 Fe1 69.1(2) . . ? C24 C23 H23A 126.2 . . ? C22 C23 H23A 126.2 . . ? Fe1 C23 H23A 126.2 . . ? C23 C24 C20 108.6(5) . . ? C23 C24 Fe1 70.4(3) . . ? C20 C24 Fe1 69.6(3) . . ? C23 C24 H24A 125.7 . . ? C20 C24 H24A 125.7 . . ? Fe1 C24 H24A 125.7 . . ? C105 C100 C101 117.5(3) . . ? C105 C100 Si1 125.7(3) . . ? C101 C100 Si1 116.7(3) . . ? C102 C101 C100 120.1(4) . . ? C102 C101 C106 117.4(3) . . ? C100 C101 C106 122.5(3) . . ? C103 C102 C101 122.5(4) . . ? C103 C102 H10A 118.8 . . ? C101 C102 H10A 118.8 . . ? C104 C103 C102 117.1(4) . . ? C104 C103 C107 121.2(5) . . ? C102 C103 C107 121.6(4) . . ? C103 C104 C105 123.3(4) . . ? C103 C104 H10B 118.4 . . ? C105 C104 H10B 118.4 . . ? C104 C105 C100 119.5(4) . . ? C104 C105 C108 116.4(3) . . ? C100 C105 C108 124.1(3) . . ? C101 C106 H10C 109.5 . . ? C101 C106 H10D 109.5 . . ? H10C C106 H10D 109.5 . . ? C101 C106 H10E 109.5 . . ? H10C C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C103 C107 H10F 109.5 . . ? C103 C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C103 C107 H10H 109.5 . . ? H10F C107 H10H 109.5 . . ? H10G C107 H10H 109.5 . . ? C105 C108 H10I 109.5 . . ? C105 C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? C105 C108 H10K 109.5 . . ? H10I C108 H10K 109.5 . . ? H10J C108 H10K 109.5 . . ? C201 C200 C205 117.5(3) . . ? C201 C200 Si1 125.8(3) . . ? C205 C200 Si1 116.7(3) . . ? C202 C201 C200 119.7(3) . . ? C202 C201 C206 116.7(3) . . ? C200 C201 C206 123.6(3) . . ? C203 C202 C201 122.9(3) . . ? C203 C202 H20B 118.6 . . ? C201 C202 H20B 118.6 . . ? C202 C203 C204 117.5(3) . . ? C202 C203 C207 121.8(4) . . ? C204 C203 C207 120.7(4) . . ? C205 C204 C203 122.0(4) . . ? C205 C204 H20C 119.0 . . ? C203 C204 H20C 119.0 . . ? C204 C205 C200 120.4(3) . . ? C204 C205 C208 118.0(3) . . ? C200 C205 C208 121.6(3) . . ? C201 C206 H20D 109.5 . . ? C201 C206 H20E 109.5 . . ? H20D C206 H20E 109.5 . . ? C201 C206 H20F 109.5 . . ? H20D C206 H20F 109.5 . . ? H20E C206 H20F 109.5 . . ? C203 C207 H20G 109.5 . . ? C203 C207 H20H 109.5 . . ? H20G C207 H20H 109.5 . . ? C203 C207 H20I 109.5 . . ? H20G C207 H20I 109.5 . . ? H20H C207 H20I 109.5 . . ? C205 C208 H20J 109.5 . . ? C205 C208 H20K 109.5 . . ? H20J C208 H20K 109.5 . . ? C205 C208 H20L 109.5 . . ? H20J C208 H20L 109.5 . . ? H20K C208 H20L 109.5 . . ? C305 C300 C301 117.0(3) . . ? C305 C300 Si2 125.2(2) . . ? C301 C300 Si2 117.7(2) . . ? C302 C301 C300 121.2(3) . . ? C302 C301 C306 116.8(3) . . ? C300 C301 C306 122.0(3) . . ? C301 C302 C303 121.4(3) . . ? C301 C302 H30A 119.3 . . ? C303 C302 H30A 119.3 . . ? C304 C303 C302 117.3(3) . . ? C304 C303 C307 121.6(4) . . ? C302 C303 C307 121.1(4) . . ? C303 C304 C305 123.4(3) . . ? C303 C304 H30B 118.3 . . ? C305 C304 H30B 118.3 . . ? C304 C305 C300 119.7(3) . . ? C304 C305 C308 116.7(3) . . ? C300 C305 C308 123.6(3) . . ? C301 C306 H30C 109.5 . . ? C301 C306 H30D 109.5 . . ? H30C C306 H30D 109.5 . . ? C301 C306 H30E 109.5 . . ? H30C C306 H30E 109.5 . . ? H30D C306 H30E 109.5 . . ? C303 C307 H30F 109.5 . . ? C303 C307 H30G 109.5 . . ? H30F C307 H30G 109.5 . . ? C303 C307 H30H 109.5 . . ? H30F C307 H30H 109.5 . . ? H30G C307 H30H 109.5 . . ? C305 C308 H30I 109.5 . . ? C305 C308 H30J 109.5 . . ? H30I C308 H30J 109.5 . . ? C305 C308 H30K 109.5 . . ? H30I C308 H30K 109.5 . . ? H30J C308 H30K 109.5 . . ? C94 C93 C98 118.0(7) . . ? C94 C93 H93A 121.0 . . ? C98 C93 H93A 121.0 . . ? C93 C94 C95 123.4(9) . . ? C93 C94 H94A 118.3 . . ? C95 C94 H94A 118.3 . . ? C96 C95 C94 118.7(10) . . ? C96 C95 H95A 120.7 . . ? C94 C95 H95A 120.7 . . ? C95 C96 C97 120.7(8) . . ? C95 C96 H96A 119.7 . . ? C97 C96 H96A 119.7 . . ? C98 C97 C96 120.4(7) . . ? C98 C97 H97A 119.8 . . ? C96 C97 H97A 119.8 . . ? C97 C98 C93 118.7(9) . . ? C97 C98 C99 122.5(9) . . ? C93 C98 C99 118.8(9) . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Ge1 Si1 C100 -75.83(14) . . . . ? Si1 Ge1 Si1 C100 65.64(13) 2_655 . . . ? Si2 Ge1 Si1 C100 154.30(13) . . . . ? Ge1 Ge1 Si1 C100 109.99(13) 2_655 . . . ? S1 Ge1 Si1 C200 58.54(13) . . . . ? Si1 Ge1 Si1 C200 -159.99(12) 2_655 . . . ? Si2 Ge1 Si1 C200 -71.33(12) . . . . ? Ge1 Ge1 Si1 C200 -115.64(12) 2_655 . . . ? S1 Ge1 Si1 Ge1 174.18(4) . . . 2_655 ? Si1 Ge1 Si1 Ge1 -44.35(4) 2_655 . . 2_655 ? Si2 Ge1 Si1 Ge1 44.32(2) . . . 2_655 ? Si1 Ge1 S1 C10 -99.32(16) 2_655 . . . ? Si2 Ge1 S1 C10 151.31(15) . . . . ? Si1 Ge1 S1 C10 31.80(16) . . . . ? S1 Ge1 Si2 C300 -74.95(11) . . . . ? Si1 Ge1 Si2 C300 156.32(11) 2_655 . . . ? Si1 Ge1 Si2 C300 67.48(11) . . . . ? Ge1 Ge1 Si2 C300 111.65(11) 2_655 . . . ? S1 Ge1 Si2 C300 59.29(12) . . . 2_655 ? Si1 Ge1 Si2 C300 -69.44(12) 2_655 . . 2_655 ? Si1 Ge1 Si2 C300 -158.28(11) . . . 2_655 ? Ge1 Ge1 Si2 C300 -114.12(11) 2_655 . . 2_655 ? S1 Ge1 Si2 Ge1 173.41(4) . . . 2_655 ? Si1 Ge1 Si2 Ge1 44.68(2) 2_655 . . 2_655 ? Si1 Ge1 Si2 Ge1 -44.16(3) . . . 2_655 ? Ge1 S1 C10 C14 91.9(4) . . . . ? Ge1 S1 C10 C11 -94.4(3) . . . . ? Ge1 S1 C10 Fe1 179.02(17) . . . . ? C12 Fe1 C10 C14 -82.7(5) . . . . ? C21 Fe1 C10 C14 149.4(3) . . . . ? C22 Fe1 C10 C14 -172.5(4) . . . . ? C20 Fe1 C10 C14 105.8(4) . . . . ? C24 Fe1 C10 C14 66.3(4) . . . . ? C13 Fe1 C10 C14 -40.5(5) . . . . ? C11 Fe1 C10 C14 -120.9(5) . . . . ? C12 Fe1 C10 C11 38.2(4) . . . . ? C14 Fe1 C10 C11 120.9(5) . . . . ? C21 Fe1 C10 C11 -89.7(3) . . . . ? C22 Fe1 C10 C11 -51.6(4) . . . . ? C20 Fe1 C10 C11 -133.3(3) . . . . ? C24 Fe1 C10 C11 -172.8(3) . . . . ? C13 Fe1 C10 C11 80.4(4) . . . . ? C12 Fe1 C10 S1 156.5(4) . . . . ? C14 Fe1 C10 S1 -120.8(4) . . . . ? C21 Fe1 C10 S1 28.6(3) . . . . ? C22 Fe1 C10 S1 66.7(4) . . . . ? C20 Fe1 C10 S1 -15.0(3) . . . . ? C24 Fe1 C10 S1 -54.5(4) . . . . ? C13 Fe1 C10 S1 -161.3(4) . . . . ? C11 Fe1 C10 S1 118.3(4) . . . . ? C14 C10 C11 C12 -0.6(5) . . . . ? S1 C10 C11 C12 -175.2(3) . . . . ? Fe1 C10 C11 C12 -58.9(3) . . . . ? C14 C10 C11 Fe1 58.3(3) . . . . ? S1 C10 C11 Fe1 -116.3(3) . . . . ? C14 Fe1 C11 C12 81.4(5) . . . . ? C21 Fe1 C11 C12 -134.7(5) . . . . ? C22 Fe1 C11 C12 -91.1(5) . . . . ? C20 Fe1 C11 C12 -172.1(4) . . . . ? C10 Fe1 C11 C12 118.1(5) . . . . ? C13 Fe1 C11 C12 36.0(4) . . . . ? C23 Fe1 C11 C12 -56.5(6) . . . . ? C12 Fe1 C11 C10 -118.1(5) . . . . ? C14 Fe1 C11 C10 -36.7(3) . . . . ? C21 Fe1 C11 C10 107.2(3) . . . . ? C22 Fe1 C11 C10 150.8(3) . . . . ? C20 Fe1 C11 C10 69.8(4) . . . . ? C13 Fe1 C11 C10 -82.0(4) . . . . ? C23 Fe1 C11 C10 -174.5(3) . . . . ? C10 C11 C12 C13 -1.4(6) . . . . ? Fe1 C11 C12 C13 -60.7(5) . . . . ? C10 C11 C12 Fe1 59.2(3) . . . . ? C14 Fe1 C12 C13 38.0(3) . . . . ? C21 Fe1 C12 C13 -173.7(3) . . . . ? C22 Fe1 C12 C13 -135.2(3) . . . . ? C24 Fe1 C12 C13 -58.3(6) . . . . ? C10 Fe1 C12 C13 81.8(4) . . . . ? C23 Fe1 C12 C13 -91.9(4) . . . . ? C11 Fe1 C12 C13 120.3(5) . . . . ? C14 Fe1 C12 C11 -82.3(4) . . . . ? C21 Fe1 C12 C11 66.0(4) . . . . ? C22 Fe1 C12 C11 104.5(4) . . . . ? C24 Fe1 C12 C11 -178.6(4) . . . . ? C10 Fe1 C12 C11 -38.5(3) . . . . ? C13 Fe1 C12 C11 -120.3(5) . . . . ? C23 Fe1 C12 C11 147.8(3) . . . . ? C11 C12 C13 C14 2.8(7) . . . . ? Fe1 C12 C13 C14 -57.6(4) . . . . ? C11 C12 C13 Fe1 60.4(4) . . . . ? C14 Fe1 C13 C12 -120.8(5) . . . . ? C22 Fe1 C13 C12 63.7(5) . . . . ? C20 Fe1 C13 C12 -176.3(4) . . . . ? C24 Fe1 C13 C12 147.4(4) . . . . ? C10 Fe1 C13 C12 -81.7(4) . . . . ? C23 Fe1 C13 C12 104.3(4) . . . . ? C11 Fe1 C13 C12 -37.4(3) . . . . ? C12 Fe1 C13 C14 120.8(5) . . . . ? C22 Fe1 C13 C14 -175.5(3) . . . . ? C20 Fe1 C13 C14 -55.5(6) . . . . ? C24 Fe1 C13 C14 -91.8(4) . . . . ? C10 Fe1 C13 C14 39.1(3) . . . . ? C23 Fe1 C13 C14 -134.9(4) . . . . ? C11 Fe1 C13 C14 83.4(4) . . . . ? C11 C10 C14 C13 2.2(5) . . . . ? S1 C10 C14 C13 176.6(3) . . . . ? Fe1 C10 C14 C13 60.9(3) . . . . ? C11 C10 C14 Fe1 -58.7(3) . . . . ? S1 C10 C14 Fe1 115.8(3) . . . . ? C12 C13 C14 C10 -3.1(6) . . . . ? Fe1 C13 C14 C10 -61.3(3) . . . . ? C12 C13 C14 Fe1 58.2(4) . . . . ? C12 Fe1 C14 C10 80.5(4) . . . . ? C21 Fe1 C14 C10 -55.5(6) . . . . ? C20 Fe1 C14 C10 -92.6(3) . . . . ? C24 Fe1 C14 C10 -136.5(3) . . . . ? C13 Fe1 C14 C10 115.9(6) . . . . ? C23 Fe1 C14 C10 -176.1(3) . . . . ? C11 Fe1 C14 C10 36.9(3) . . . . ? C12 Fe1 C14 C13 -35.4(4) . . . . ? C21 Fe1 C14 C13 -171.4(5) . . . . ? C20 Fe1 C14 C13 151.5(5) . . . . ? C24 Fe1 C14 C13 107.7(5) . . . . ? C10 Fe1 C14 C13 -115.9(6) . . . . ? C23 Fe1 C14 C13 68.0(6) . . . . ? C11 Fe1 C14 C13 -79.0(5) . . . . ? C14 Fe1 C20 C21 148.6(3) . . . . ? C22 Fe1 C20 C21 -37.9(3) . . . . ? C24 Fe1 C20 C21 -119.1(4) . . . . ? C10 Fe1 C20 C21 104.4(3) . . . . ? C13 Fe1 C20 C21 -173.6(4) . . . . ? C23 Fe1 C20 C21 -82.0(3) . . . . ? C11 Fe1 C20 C21 63.4(4) . . . . ? C14 Fe1 C20 C24 -92.3(4) . . . . ? C21 Fe1 C20 C24 119.1(4) . . . . ? C22 Fe1 C20 C24 81.2(3) . . . . ? C10 Fe1 C20 C24 -136.4(3) . . . . ? C13 Fe1 C20 C24 -54.5(5) . . . . ? C23 Fe1 C20 C24 37.1(3) . . . . ? C11 Fe1 C20 C24 -177.5(3) . . . . ? C24 C20 C21 C22 -0.3(5) . . . . ? Fe1 C20 C21 C22 59.4(3) . . . . ? C24 C20 C21 Fe1 -59.7(3) . . . . ? C12 Fe1 C21 C20 -175.7(3) . . . . ? C14 Fe1 C21 C20 -57.1(5) . . . . ? C22 Fe1 C21 C20 119.3(4) . . . . ? C24 Fe1 C21 C20 37.7(3) . . . . ? C10 Fe1 C21 C20 -93.4(3) . . . . ? C23 Fe1 C21 C20 81.0(3) . . . . ? C11 Fe1 C21 C20 -137.0(3) . . . . ? C12 Fe1 C21 C22 65.0(4) . . . . ? C14 Fe1 C21 C22 -176.4(4) . . . . ? C20 Fe1 C21 C22 -119.3(4) . . . . ? C24 Fe1 C21 C22 -81.6(3) . . . . ? C10 Fe1 C21 C22 147.3(3) . . . . ? C23 Fe1 C21 C22 -38.2(3) . . . . ? C11 Fe1 C21 C22 103.7(3) . . . . ? C20 C21 C22 C23 0.7(5) . . . . ? Fe1 C21 C22 C23 60.3(3) . . . . ? C20 C21 C22 Fe1 -59.6(3) . . . . ? C12 Fe1 C22 C21 -135.4(4) . . . . ? C20 Fe1 C22 C21 37.3(3) . . . . ? C24 Fe1 C22 C21 81.0(3) . . . . ? C10 Fe1 C22 C21 -58.6(4) . . . . ? C13 Fe1 C22 C21 -171.7(4) . . . . ? C23 Fe1 C22 C21 118.3(4) . . . . ? C11 Fe1 C22 C21 -92.3(3) . . . . ? C12 Fe1 C22 C23 106.4(4) . . . . ? C21 Fe1 C22 C23 -118.3(4) . . . . ? C20 Fe1 C22 C23 -81.0(3) . . . . ? C24 Fe1 C22 C23 -37.3(3) . . . . ? C10 Fe1 C22 C23 -176.8(3) . . . . ? C13 Fe1 C22 C23 70.0(5) . . . . ? C11 Fe1 C22 C23 149.4(3) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? Fe1 C22 C23 C24 59.1(3) . . . . ? C21 C22 C23 Fe1 -59.8(3) . . . . ? C12 Fe1 C23 C24 150.9(4) . . . . ? C14 Fe1 C23 C24 67.9(4) . . . . ? C21 Fe1 C23 C24 -80.9(3) . . . . ? C22 Fe1 C23 C24 -119.3(4) . . . . ? C20 Fe1 C23 C24 -37.5(3) . . . . ? C13 Fe1 C23 C24 109.1(4) . . . . ? C11 Fe1 C23 C24 -172.7(4) . . . . ? C12 Fe1 C23 C22 -89.8(4) . . . . ? C14 Fe1 C23 C22 -172.8(3) . . . . ? C21 Fe1 C23 C22 38.3(3) . . . . ? C20 Fe1 C23 C22 81.8(3) . . . . ? C24 Fe1 C23 C22 119.3(4) . . . . ? C13 Fe1 C23 C22 -131.7(4) . . . . ? C11 Fe1 C23 C22 -53.4(5) . . . . ? C22 C23 C24 C20 0.6(5) . . . . ? Fe1 C23 C24 C20 59.3(3) . . . . ? C22 C23 C24 Fe1 -58.8(3) . . . . ? C21 C20 C24 C23 -0.1(5) . . . . ? Fe1 C20 C24 C23 -59.8(3) . . . . ? C21 C20 C24 Fe1 59.6(3) . . . . ? C12 Fe1 C24 C23 -51.8(6) . . . . ? C14 Fe1 C24 C23 -134.4(3) . . . . ? C21 Fe1 C24 C23 82.2(3) . . . . ? C22 Fe1 C24 C23 37.9(3) . . . . ? C20 Fe1 C24 C23 119.6(5) . . . . ? C10 Fe1 C24 C23 -174.1(3) . . . . ? C13 Fe1 C24 C23 -88.7(4) . . . . ? C12 Fe1 C24 C20 -171.4(5) . . . . ? C14 Fe1 C24 C20 105.9(3) . . . . ? C21 Fe1 C24 C20 -37.5(3) . . . . ? C22 Fe1 C24 C20 -81.7(3) . . . . ? C10 Fe1 C24 C20 66.3(4) . . . . ? C13 Fe1 C24 C20 151.6(4) . . . . ? C23 Fe1 C24 C20 -119.6(5) . . . . ? C200 Si1 C100 C105 -112.8(3) . . . . ? Ge1 Si1 C100 C105 108.6(3) 2_655 . . . ? Ge1 Si1 C100 C105 24.6(4) . . . . ? C200 Si1 C100 C101 65.6(3) . . . . ? Ge1 Si1 C100 C101 -73.0(3) 2_655 . . . ? Ge1 Si1 C100 C101 -157.0(2) . . . . ? C105 C100 C101 C102 -0.9(6) . . . . ? Si1 C100 C101 C102 -179.4(4) . . . . ? C105 C100 C101 C106 -179.8(4) . . . . ? Si1 C100 C101 C106 1.7(5) . . . . ? C100 C101 C102 C103 0.3(7) . . . . ? C106 C101 C102 C103 179.3(5) . . . . ? C101 C102 C103 C104 -0.3(8) . . . . ? C101 C102 C103 C107 -178.5(6) . . . . ? C102 C103 C104 C105 0.8(8) . . . . ? C107 C103 C104 C105 179.0(6) . . . . ? C103 C104 C105 C100 -1.4(7) . . . . ? C103 C104 C105 C108 179.1(5) . . . . ? C101 C100 C105 C104 1.4(6) . . . . ? Si1 C100 C105 C104 179.8(3) . . . . ? C101 C100 C105 C108 -179.1(4) . . . . ? Si1 C100 C105 C108 -0.7(5) . . . . ? C100 Si1 C200 C201 -111.2(3) . . . . ? Ge1 Si1 C200 C201 25.1(3) 2_655 . . . ? Ge1 Si1 C200 C201 109.4(3) . . . . ? C100 Si1 C200 C205 65.7(3) . . . . ? Ge1 Si1 C200 C205 -158.0(2) 2_655 . . . ? Ge1 Si1 C200 C205 -73.7(3) . . . . ? C205 C200 C201 C202 0.5(5) . . . . ? Si1 C200 C201 C202 177.3(3) . . . . ? C205 C200 C201 C206 179.3(3) . . . . ? Si1 C200 C201 C206 -3.8(5) . . . . ? C200 C201 C202 C203 0.8(5) . . . . ? C206 C201 C202 C203 -178.2(3) . . . . ? C201 C202 C203 C204 -0.3(6) . . . . ? C201 C202 C203 C207 178.9(4) . . . . ? C202 C203 C204 C205 -1.4(6) . . . . ? C207 C203 C204 C205 179.4(4) . . . . ? C203 C204 C205 C200 2.7(6) . . . . ? C203 C204 C205 C208 -178.7(4) . . . . ? C201 C200 C205 C204 -2.1(5) . . . . ? Si1 C200 C205 C204 -179.2(3) . . . . ? C201 C200 C205 C208 179.4(3) . . . . ? Si1 C200 C205 C208 2.2(5) . . . . ? C300 Si2 C300 C305 -117.6(3) 2_655 . . . ? Ge1 Si2 C300 C305 104.1(3) 2_655 . . . ? Ge1 Si2 C300 C305 19.8(3) . . . . ? C300 Si2 C300 C301 62.0(2) 2_655 . . . ? Ge1 Si2 C300 C301 -76.4(3) 2_655 . . . ? Ge1 Si2 C300 C301 -160.6(2) . . . . ? C305 C300 C301 C302 -0.6(5) . . . . ? Si2 C300 C301 C302 179.8(3) . . . . ? C305 C300 C301 C306 -179.5(3) . . . . ? Si2 C300 C301 C306 0.9(4) . . . . ? C300 C301 C302 C303 -0.9(5) . . . . ? C306 C301 C302 C303 178.0(3) . . . . ? C301 C302 C303 C304 1.0(5) . . . . ? C301 C302 C303 C307 -179.8(3) . . . . ? C302 C303 C304 C305 0.5(5) . . . . ? C307 C303 C304 C305 -178.7(3) . . . . ? C303 C304 C305 C300 -2.1(5) . . . . ? C303 C304 C305 C308 176.0(3) . . . . ? C301 C300 C305 C304 2.0(5) . . . . ? Si2 C300 C305 C304 -178.4(2) . . . . ? C301 C300 C305 C308 -175.9(3) . . . . ? Si2 C300 C305 C308 3.7(5) . . . . ? C98 C93 C94 C95 -3.0(16) . . . . ? C93 C94 C95 C96 0.1(16) . . . . ? C94 C95 C96 C97 3.1(13) . . . . ? C95 C96 C97 C98 -3.5(11) . . . . ? C96 C97 C98 C93 0.5(11) . . . . ? C96 C97 C98 C99 -178.7(7) . . . . ? C94 C93 C98 C97 2.5(12) . . . . ? C94 C93 C98 C99 -178.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.073 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.087 #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_5 _chemical_name_systematic ; [FcS(Sn2Si3Mes6)SFc] ; _publ_section_exptl_refinement ; ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H84 Fe2 S2 Si3 Sn2, 2(C7 H8)' _chemical_formula_sum 'C88 H100 Fe2 S2 Si3 Sn2' _chemical_formula_weight 1655.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 23.325(5) _cell_length_b 15.972(3) _cell_length_c 21.830(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.00(3) _cell_angle_gamma 90.00 _cell_volume 7734(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 28360 _cell_measurement_theta_min 3.79 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28360 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7567 _reflns_number_gt 5561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep 32' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7567 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _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 Sn1 Sn 0.558672(11) 0.348636(17) 0.229779(12) 0.02718(10) Uani 1 1 d . . . Si1 Si 0.5000 0.47956(10) 0.2500 0.0273(3) Uani 1 2 d S . . Fe2 Fe 0.77046(3) 0.27549(4) 0.19239(4) 0.0500(2) Uani 1 1 d . . . S2 S 0.64310(5) 0.37011(7) 0.18765(6) 0.0412(3) Uani 1 1 d . . . Si4 Si 0.54513(5) 0.28258(7) 0.33496(5) 0.0290(2) Uani 1 1 d . . . C10 C 0.69245(18) 0.2865(3) 0.2144(2) 0.0408(11) Uani 1 1 d . . . C11 C 0.7422(2) 0.2863(5) 0.2711(3) 0.0723(19) Uani 1 1 d . . . H11A H 0.7533 0.3321 0.3039 0.087 Uiso 1 1 calc R . . C12 C 0.7730(3) 0.2118(6) 0.2731(5) 0.113(3) Uani 1 1 d . . . H12A H 0.8105 0.1952 0.3078 0.135 Uiso 1 1 calc R . . C13 C 0.7440(4) 0.1641(4) 0.2203(6) 0.110(4) Uani 1 1 d . . . H13A H 0.7569 0.1074 0.2102 0.132 Uiso 1 1 calc R . . C14 C 0.6929(2) 0.2115(3) 0.1802(3) 0.0725(18) Uani 1 1 d . . . H14A H 0.6631 0.1935 0.1386 0.087 Uiso 1 1 calc R . . C20 C 0.8038(2) 0.3865(3) 0.1757(3) 0.0559(13) Uani 1 1 d . . . H20A H 0.7967 0.4417 0.1937 0.067 Uiso 1 1 calc R . . C21 C 0.8511(2) 0.3297(3) 0.2049(3) 0.0573(14) Uani 1 1 d . . . H21A H 0.8834 0.3380 0.2470 0.069 Uiso 1 1 calc R . . C22 C 0.8454(2) 0.2614(3) 0.1643(3) 0.0543(13) Uani 1 1 d . . . H22A H 0.8724 0.2112 0.1724 0.065 Uiso 1 1 calc R . . C23 C 0.7944(3) 0.2742(4) 0.1102(3) 0.0640(15) Uani 1 1 d . . . H23A H 0.7789 0.2348 0.0732 0.077 Uiso 1 1 calc R . . C24 C 0.7690(2) 0.3521(3) 0.1174(3) 0.0604(15) Uani 1 1 d . . . H24A H 0.7324 0.3779 0.0864 0.072 Uiso 1 1 calc R . . C100 C 0.54512(17) 0.1648(2) 0.34351(19) 0.0317(9) Uani 1 1 d . . . C101 C 0.5155(2) 0.1312(3) 0.3857(2) 0.0405(11) Uani 1 1 d . . . C102 C 0.5133(2) 0.0456(3) 0.3938(3) 0.0567(13) Uani 1 1 d . . . H10A H 0.4936 0.0245 0.4227 0.068 Uiso 1 1 calc R . . C103 C 0.5388(3) -0.0106(3) 0.3615(3) 0.0630(15) Uani 1 1 d . . . C104 C 0.5672(2) 0.0226(3) 0.3202(2) 0.0541(13) Uani 1 1 d . . . H10B H 0.5845 -0.0148 0.2971 0.065 Uiso 1 1 calc R . . C105 C 0.57163(18) 0.1071(3) 0.3110(2) 0.0394(10) Uani 1 1 d . . . C106 C 0.4850(2) 0.1856(3) 0.4222(2) 0.0453(11) Uani 1 1 d . . . H10C H 0.4641 0.1503 0.4454 0.068 Uiso 1 1 calc R . . H10D H 0.4557 0.2220 0.3921 0.068 Uiso 1 1 calc R . . H10E H 0.5152 0.2201 0.4531 0.068 Uiso 1 1 calc R . . C107 C 0.5347(3) -0.1035(4) 0.3706(4) 0.103(3) Uani 1 1 d . . . H10F H 0.5749 -0.1284 0.3803 0.154 Uiso 1 1 calc R . . H10G H 0.5079 -0.1284 0.3310 0.154 Uiso 1 1 calc R . . H10H H 0.5186 -0.1142 0.4063 0.154 Uiso 1 1 calc R . . C108 C 0.6045(2) 0.1331(3) 0.2648(2) 0.0448(11) Uani 1 1 d . . . H10I H 0.6295 0.0865 0.2585 0.067 Uiso 1 1 calc R . . H10J H 0.6303 0.1814 0.2824 0.067 Uiso 1 1 calc R . . H10K H 0.5753 0.1483 0.2234 0.067 Uiso 1 1 calc R . . C200 C 0.59098(18) 0.3333(3) 0.41350(18) 0.0312(9) Uani 1 1 d . . . C201 C 0.56753(19) 0.3826(3) 0.45340(19) 0.0361(10) Uani 1 1 d . . . C202 C 0.6054(2) 0.4143(3) 0.51070(19) 0.0396(10) Uani 1 1 d . . . H20B H 0.5885 0.4465 0.5374 0.047 Uiso 1 1 calc R . . C203 C 0.6667(2) 0.4008(3) 0.5303(2) 0.0436(11) Uani 1 1 d . . . C204 C 0.6899(2) 0.3528(3) 0.4905(2) 0.0424(11) Uani 1 1 d . . . H20C H 0.7322 0.3437 0.5027 0.051 Uiso 1 1 calc R . . C205 C 0.65398(18) 0.3180(3) 0.43394(19) 0.0365(10) Uani 1 1 d . . . C206 C 0.50184(18) 0.4065(3) 0.43601(19) 0.0379(10) Uani 1 1 d . . . H20D H 0.4922 0.4220 0.4751 0.057 Uiso 1 1 calc R . . H20E H 0.4768 0.3589 0.4153 0.057 Uiso 1 1 calc R . . H20F H 0.4939 0.4542 0.4063 0.057 Uiso 1 1 calc R . . C207 C 0.7075(2) 0.4363(4) 0.5922(2) 0.0641(15) Uani 1 1 d . . . H20G H 0.6838 0.4708 0.6127 0.096 Uiso 1 1 calc R . . H20H H 0.7386 0.4710 0.5830 0.096 Uiso 1 1 calc R . . H20I H 0.7267 0.3905 0.6211 0.096 Uiso 1 1 calc R . . C208 C 0.68344(19) 0.2665(3) 0.3945(2) 0.0438(11) Uani 1 1 d . . . H20J H 0.7273 0.2697 0.4134 0.066 Uiso 1 1 calc R . . H20K H 0.6717 0.2880 0.3503 0.066 Uiso 1 1 calc R . . H20L H 0.6705 0.2080 0.3941 0.066 Uiso 1 1 calc R . . C300 C 0.53710(17) 0.5464(2) 0.32378(18) 0.0286(8) Uani 1 1 d . . . C301 C 0.49969(18) 0.5988(3) 0.34678(18) 0.0332(9) Uani 1 1 d . . . C302 C 0.5234(2) 0.6475(3) 0.40162(19) 0.0367(10) Uani 1 1 d . . . H30A H 0.4974 0.6831 0.4158 0.044 Uiso 1 1 calc R . . C303 C 0.5841(2) 0.6451(3) 0.4358(2) 0.0390(10) Uani 1 1 d . . . C304 C 0.62027(19) 0.5933(3) 0.41352(18) 0.0368(10) Uani 1 1 d . . . H30B H 0.6619 0.5904 0.4372 0.044 Uiso 1 1 calc R . . C305 C 0.59930(17) 0.5449(3) 0.35833(17) 0.0308(9) Uani 1 1 d . . . C306 C 0.43252(19) 0.6033(3) 0.3147(2) 0.0460(11) Uani 1 1 d . . . H30C H 0.4146 0.6414 0.3389 0.069 Uiso 1 1 calc R . . H30D H 0.4150 0.5474 0.3137 0.069 Uiso 1 1 calc R . . H30E H 0.4243 0.6240 0.2705 0.069 Uiso 1 1 calc R . . C307 C 0.6096(2) 0.6984(3) 0.4950(2) 0.0537(13) Uani 1 1 d . . . H30F H 0.6470 0.7250 0.4934 0.081 Uiso 1 1 calc R . . H30G H 0.6182 0.6631 0.5336 0.081 Uiso 1 1 calc R . . H30H H 0.5803 0.7416 0.4966 0.081 Uiso 1 1 calc R . . C308 C 0.64511(17) 0.4965(3) 0.3379(2) 0.0371(10) Uani 1 1 d . . . H30I H 0.6856 0.5119 0.3651 0.056 Uiso 1 1 calc R . . H30J H 0.6410 0.5094 0.2928 0.056 Uiso 1 1 calc R . . H30K H 0.6388 0.4364 0.3423 0.056 Uiso 1 1 calc R . . C93 C 0.6502(4) 0.0090(5) 0.6011(4) 0.106(3) Uani 1 1 d . . . H93A H 0.6586 -0.0451 0.6199 0.128 Uiso 1 1 calc R . . C94 C 0.6290(5) 0.0698(5) 0.6315(4) 0.138(4) Uani 1 1 d . . . H94A H 0.6217 0.0569 0.6709 0.165 Uiso 1 1 calc R . . C95 C 0.6178(4) 0.1492(5) 0.6074(4) 0.102(3) Uani 1 1 d . . . H95A H 0.6030 0.1911 0.6295 0.123 Uiso 1 1 calc R . . C96 C 0.6278(3) 0.1657(6) 0.5538(4) 0.097(3) Uani 1 1 d . . . H96A H 0.6218 0.2212 0.5375 0.117 Uiso 1 1 calc R . . C97 C 0.6471(3) 0.1045(6) 0.5192(4) 0.097(2) Uani 1 1 d . . . H97A H 0.6516 0.1181 0.4786 0.116 Uiso 1 1 calc R . . C98 C 0.6597(3) 0.0253(5) 0.5428(4) 0.091(2) Uani 1 1 d . . . C99 C 0.6807(4) -0.0405(7) 0.5086(5) 0.152(4) Uani 1 1 d . . . H99A H 0.7191 -0.0237 0.5029 0.228 Uiso 1 1 calc R . . H99B H 0.6508 -0.0495 0.4663 0.228 Uiso 1 1 calc R . . H99C H 0.6863 -0.0925 0.5336 0.228 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 Sn1 0.02583(16) 0.02824(17) 0.02972(17) -0.00035(11) 0.01185(11) -0.00001(11) Si1 0.0254(7) 0.0271(8) 0.0299(8) 0.000 0.0090(6) 0.000 Fe2 0.0392(4) 0.0422(4) 0.0812(5) 0.0143(4) 0.0371(4) 0.0073(3) S2 0.0370(6) 0.0427(7) 0.0524(7) 0.0049(5) 0.0264(5) 0.0010(5) Si4 0.0298(6) 0.0297(6) 0.0287(5) 0.0024(5) 0.0110(4) 0.0030(5) C10 0.027(2) 0.041(3) 0.061(3) 0.014(2) 0.025(2) 0.0024(19) C11 0.036(3) 0.122(6) 0.069(4) 0.037(4) 0.030(3) 0.012(3) C12 0.062(4) 0.126(7) 0.173(8) 0.103(7) 0.070(5) 0.038(5) C13 0.080(5) 0.043(4) 0.250(12) 0.045(5) 0.117(7) 0.022(3) C14 0.054(3) 0.045(3) 0.144(6) -0.006(3) 0.069(4) -0.002(3) C20 0.057(3) 0.039(3) 0.088(4) 0.001(3) 0.047(3) 0.002(2) C21 0.043(3) 0.064(4) 0.075(4) 0.002(3) 0.034(3) -0.015(3) C22 0.045(3) 0.053(3) 0.078(4) 0.003(3) 0.040(3) 0.008(2) C23 0.069(4) 0.060(4) 0.073(4) -0.001(3) 0.036(3) -0.005(3) C24 0.049(3) 0.059(4) 0.075(4) 0.026(3) 0.021(3) 0.004(3) C100 0.030(2) 0.029(2) 0.037(2) 0.0037(17) 0.0123(17) 0.0020(17) C101 0.043(3) 0.039(3) 0.045(3) 0.010(2) 0.023(2) 0.008(2) C102 0.069(3) 0.040(3) 0.077(3) 0.019(3) 0.046(3) 0.006(3) C103 0.069(4) 0.034(3) 0.098(4) 0.011(3) 0.043(3) 0.011(3) C104 0.060(3) 0.035(3) 0.078(3) 0.004(3) 0.036(3) 0.011(2) C105 0.031(2) 0.037(3) 0.054(3) 0.004(2) 0.020(2) 0.0083(19) C106 0.060(3) 0.039(3) 0.050(3) 0.009(2) 0.035(2) 0.003(2) C107 0.132(6) 0.038(3) 0.183(7) 0.024(4) 0.115(6) 0.010(4) C108 0.044(3) 0.045(3) 0.051(3) -0.003(2) 0.023(2) 0.007(2) C200 0.033(2) 0.035(2) 0.0254(19) 0.0060(17) 0.0081(16) 0.0006(17) C201 0.044(2) 0.031(2) 0.036(2) 0.0065(18) 0.0178(19) 0.0014(19) C202 0.054(3) 0.036(2) 0.029(2) 0.0013(19) 0.0132(19) 0.002(2) C203 0.055(3) 0.038(3) 0.032(2) 0.004(2) 0.006(2) -0.007(2) C204 0.036(2) 0.045(3) 0.041(2) 0.005(2) 0.005(2) -0.002(2) C205 0.037(2) 0.039(2) 0.031(2) 0.0056(19) 0.0082(18) 0.0009(19) C206 0.046(3) 0.040(3) 0.035(2) 0.0018(19) 0.0234(19) 0.005(2) C207 0.068(4) 0.061(4) 0.054(3) -0.003(3) 0.005(3) -0.016(3) C208 0.035(2) 0.053(3) 0.042(2) 0.002(2) 0.0089(19) 0.011(2) C300 0.031(2) 0.024(2) 0.033(2) -0.0006(16) 0.0126(16) -0.0013(16) C301 0.039(2) 0.031(2) 0.030(2) 0.0033(17) 0.0102(17) -0.0008(18) C302 0.049(3) 0.031(2) 0.034(2) -0.0059(18) 0.0188(19) -0.0046(19) C303 0.049(3) 0.036(2) 0.032(2) 0.0004(19) 0.014(2) -0.009(2) C304 0.038(2) 0.039(3) 0.031(2) 0.0001(19) 0.0073(18) -0.007(2) C305 0.033(2) 0.030(2) 0.029(2) 0.0028(17) 0.0094(16) -0.0042(17) C306 0.041(3) 0.048(3) 0.048(3) -0.009(2) 0.013(2) 0.012(2) C307 0.058(3) 0.065(4) 0.040(3) -0.017(2) 0.018(2) -0.011(3) C308 0.029(2) 0.037(2) 0.044(2) -0.0020(19) 0.0099(18) -0.0019(18) C93 0.173(8) 0.058(4) 0.087(5) 0.007(4) 0.039(5) -0.013(5) C94 0.253(12) 0.072(6) 0.094(6) 0.013(5) 0.063(7) -0.001(7) C95 0.129(7) 0.069(5) 0.103(6) 0.007(4) 0.029(5) -0.008(4) C96 0.068(4) 0.107(7) 0.103(6) 0.054(5) 0.005(4) -0.011(4) C97 0.065(4) 0.126(7) 0.097(5) 0.045(5) 0.022(4) 0.008(5) C98 0.065(4) 0.105(6) 0.095(5) 0.005(5) 0.014(4) -0.003(4) C99 0.114(7) 0.172(10) 0.174(9) -0.047(8) 0.049(7) 0.018(7) _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 Sn1 S2 2.4414(12) . ? Sn1 Si1 2.6103(13) . ? Sn1 Si4 2.6186(13) 2_655 ? Sn1 Si4 2.6332(12) . ? Sn1 Sn1 3.1248(8) 2_655 ? Si1 C300 1.903(4) 2_655 ? Si1 C300 1.903(4) . ? Si1 Sn1 2.6103(13) 2_655 ? Fe2 C21 2.012(5) . ? Fe2 C20 2.013(5) . ? Fe2 C12 2.019(7) . ? Fe2 C14 2.022(5) . ? Fe2 C10 2.027(4) . ? Fe2 C11 2.029(5) . ? Fe2 C24 2.036(5) . ? Fe2 C22 2.036(5) . ? Fe2 C13 2.038(6) . ? Fe2 C23 2.039(5) . ? S2 C10 1.742(4) . ? Si4 C100 1.891(4) . ? Si4 C200 1.899(4) . ? Si4 Sn1 2.6186(13) 2_655 ? C10 C11 1.411(7) . ? C10 C14 1.412(7) . ? C11 C12 1.384(10) . ? C11 H11A 1.0000 . ? C12 C13 1.373(11) . ? C12 H12A 1.0000 . ? C13 C14 1.455(10) . ? C13 H13A 1.0000 . ? C14 H14A 1.0000 . ? C20 C24 1.393(7) . ? C20 C21 1.419(7) . ? C20 H20A 1.0000 . ? C21 C22 1.385(7) . ? C21 H21A 1.0000 . ? C22 C23 1.409(7) . ? C22 H22A 1.0000 . ? C23 C24 1.408(7) . ? C23 H23A 1.0000 . ? C24 H24A 1.0000 . ? C100 C101 1.415(6) . ? C100 C105 1.416(6) . ? C101 C102 1.381(6) . ? C101 C106 1.501(6) . ? C102 C103 1.385(7) . ? C102 H10A 0.9500 . ? C103 C104 1.377(7) . ? C103 C107 1.504(7) . ? C104 C105 1.373(6) . ? C104 H10B 0.9500 . ? C105 C108 1.502(6) . ? C106 H10C 0.9800 . ? C106 H10D 0.9800 . ? C106 H10E 0.9800 . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? C107 H10H 0.9800 . ? C108 H10I 0.9800 . ? C108 H10J 0.9800 . ? C108 H10K 0.9800 . ? C200 C201 1.405(6) . ? C200 C205 1.418(6) . ? C201 C202 1.385(6) . ? C201 C206 1.509(6) . ? C202 C203 1.377(6) . ? C202 H20B 0.9500 . ? C203 C204 1.387(6) . ? C203 C207 1.503(6) . ? C204 C205 1.376(6) . ? C204 H20C 0.9500 . ? C205 C208 1.502(6) . ? C206 H20D 0.9800 . ? C206 H20E 0.9800 . ? C206 H20F 0.9800 . ? C207 H20G 0.9800 . ? C207 H20H 0.9800 . ? C207 H20I 0.9800 . ? C208 H20J 0.9800 . ? C208 H20K 0.9800 . ? C208 H20L 0.9800 . ? C300 C301 1.409(5) . ? C300 C305 1.414(5) . ? C301 C302 1.391(5) . ? C301 C306 1.507(6) . ? C302 C303 1.381(6) . ? C302 H30A 0.9500 . ? C303 C304 1.374(6) . ? C303 C307 1.509(6) . ? C304 C305 1.387(5) . ? C304 H30B 0.9500 . ? C305 C308 1.494(5) . ? C306 H30C 0.9800 . ? C306 H30D 0.9800 . ? C306 H30E 0.9800 . ? C307 H30F 0.9800 . ? C307 H30G 0.9800 . ? C307 H30H 0.9800 . ? C308 H30I 0.9800 . ? C308 H30J 0.9800 . ? C308 H30K 0.9800 . ? C93 C94 1.353(11) . ? C93 C98 1.382(9) . ? C93 H93A 0.9500 . ? C94 C95 1.368(10) . ? C94 H94A 0.9500 . ? C95 C96 1.288(10) . ? C95 H95A 0.9500 . ? C96 C97 1.392(11) . ? C96 H96A 0.9500 . ? C97 C98 1.364(10) . ? C97 H97A 0.9500 . ? C98 C99 1.460(11) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Sn1 Si1 118.50(4) . . ? S2 Sn1 Si4 124.90(4) . 2_655 ? Si1 Sn1 Si4 88.19(3) . 2_655 ? S2 Sn1 Si4 135.47(4) . . ? Si1 Sn1 Si4 87.88(3) . . ? Si4 Sn1 Si4 88.23(5) 2_655 . ? S2 Sn1 Sn1 170.17(3) . 2_655 ? Si1 Sn1 Sn1 53.23(2) . 2_655 ? Si4 Sn1 Sn1 53.70(3) 2_655 2_655 ? Si4 Sn1 Sn1 53.27(3) . 2_655 ? C300 Si1 C300 111.8(2) 2_655 . ? C300 Si1 Sn1 117.87(12) 2_655 2_655 ? C300 Si1 Sn1 115.55(12) . 2_655 ? C300 Si1 Sn1 115.55(12) 2_655 . ? C300 Si1 Sn1 117.87(12) . . ? Sn1 Si1 Sn1 73.53(4) 2_655 . ? C21 Fe2 C20 41.3(2) . . ? C21 Fe2 C12 108.9(3) . . ? C20 Fe2 C12 133.8(4) . . ? C21 Fe2 C14 175.1(2) . . ? C20 Fe2 C14 143.2(2) . . ? C12 Fe2 C14 69.2(3) . . ? C21 Fe2 C10 143.2(2) . . ? C20 Fe2 C10 113.03(19) . . ? C12 Fe2 C10 67.9(2) . . ? C14 Fe2 C10 40.82(19) . . ? C21 Fe2 C11 112.6(2) . . ? C20 Fe2 C11 108.8(3) . . ? C12 Fe2 C11 40.0(3) . . ? C14 Fe2 C11 69.1(3) . . ? C10 Fe2 C11 40.70(18) . . ? C21 Fe2 C24 68.5(2) . . ? C20 Fe2 C24 40.2(2) . . ? C12 Fe2 C24 173.3(4) . . ? C14 Fe2 C24 114.0(3) . . ? C10 Fe2 C24 110.2(2) . . ? C11 Fe2 C24 134.5(3) . . ? C21 Fe2 C22 40.0(2) . . ? C20 Fe2 C22 68.1(2) . . ? C12 Fe2 C22 114.3(2) . . ? C14 Fe2 C22 136.1(2) . . ? C10 Fe2 C22 176.1(2) . . ? C11 Fe2 C22 143.0(2) . . ? C24 Fe2 C22 68.1(2) . . ? C21 Fe2 C13 133.8(3) . . ? C20 Fe2 C13 173.0(4) . . ? C12 Fe2 C13 39.6(3) . . ? C14 Fe2 C13 42.0(3) . . ? C10 Fe2 C13 68.2(2) . . ? C11 Fe2 C13 67.2(3) . . ? C24 Fe2 C13 146.5(4) . . ? C22 Fe2 C13 111.2(2) . . ? C21 Fe2 C23 67.9(2) . . ? C20 Fe2 C23 67.8(2) . . ? C12 Fe2 C23 145.2(3) . . ? C14 Fe2 C23 110.9(3) . . ? C10 Fe2 C23 136.0(2) . . ? C11 Fe2 C23 174.7(2) . . ? C24 Fe2 C23 40.4(2) . . ? C22 Fe2 C23 40.4(2) . . ? C13 Fe2 C23 116.5(3) . . ? C10 S2 Sn1 107.03(14) . . ? C100 Si4 C200 110.63(17) . . ? C100 Si4 Sn1 115.21(13) . 2_655 ? C200 Si4 Sn1 118.97(13) . 2_655 ? C100 Si4 Sn1 119.24(13) . . ? C200 Si4 Sn1 115.51(13) . . ? Sn1 Si4 Sn1 73.02(4) 2_655 . ? C11 C10 C14 108.9(5) . . ? C11 C10 S2 125.0(4) . . ? C14 C10 S2 125.8(4) . . ? C11 C10 Fe2 69.7(3) . . ? C14 C10 Fe2 69.4(3) . . ? S2 C10 Fe2 122.4(2) . . ? C12 C11 C10 107.9(7) . . ? C12 C11 Fe2 69.6(4) . . ? C10 C11 Fe2 69.6(3) . . ? C12 C11 H11A 126.0 . . ? C10 C11 H11A 126.0 . . ? Fe2 C11 H11A 126.0 . . ? C13 C12 C11 109.5(7) . . ? C13 C12 Fe2 71.0(5) . . ? C11 C12 Fe2 70.4(4) . . ? C13 C12 H12A 125.2 . . ? C11 C12 H12A 125.2 . . ? Fe2 C12 H12A 125.2 . . ? C12 C13 C14 108.4(6) . . ? C12 C13 Fe2 69.5(4) . . ? C14 C13 Fe2 68.4(3) . . ? C12 C13 H13A 125.8 . . ? C14 C13 H13A 125.8 . . ? Fe2 C13 H13A 125.8 . . ? C10 C14 C13 105.2(6) . . ? C10 C14 Fe2 69.8(3) . . ? C13 C14 Fe2 69.6(3) . . ? C10 C14 H14A 127.3 . . ? C13 C14 H14A 127.3 . . ? Fe2 C14 H14A 127.3 . . ? C24 C20 C21 108.1(5) . . ? C24 C20 Fe2 70.8(3) . . ? C21 C20 Fe2 69.3(3) . . ? C24 C20 H20A 125.9 . . ? C21 C20 H20A 125.9 . . ? Fe2 C20 H20A 125.9 . . ? C22 C21 C20 107.9(5) . . ? C22 C21 Fe2 70.9(3) . . ? C20 C21 Fe2 69.4(3) . . ? C22 C21 H21A 126.0 . . ? C20 C21 H21A 126.0 . . ? Fe2 C21 H21A 126.0 . . ? C21 C22 C23 108.2(5) . . ? C21 C22 Fe2 69.0(3) . . ? C23 C22 Fe2 69.9(3) . . ? C21 C22 H22A 125.9 . . ? C23 C22 H22A 125.9 . . ? Fe2 C22 H22A 125.9 . . ? C24 C23 C22 108.1(5) . . ? C24 C23 Fe2 69.7(3) . . ? C22 C23 Fe2 69.7(3) . . ? C24 C23 H23A 126.0 . . ? C22 C23 H23A 126.0 . . ? Fe2 C23 H23A 126.0 . . ? C20 C24 C23 107.7(5) . . ? C20 C24 Fe2 69.0(3) . . ? C23 C24 Fe2 69.9(3) . . ? C20 C24 H24A 126.2 . . ? C23 C24 H24A 126.2 . . ? Fe2 C24 H24A 126.2 . . ? C101 C100 C105 117.1(4) . . ? C101 C100 Si4 117.1(3) . . ? C105 C100 Si4 125.7(3) . . ? C102 C101 C100 120.2(4) . . ? C102 C101 C106 117.6(4) . . ? C100 C101 C106 122.2(4) . . ? C101 C102 C103 122.5(5) . . ? C101 C102 H10A 118.7 . . ? C103 C102 H10A 118.7 . . ? C104 C103 C102 116.8(5) . . ? C104 C103 C107 122.0(5) . . ? C102 C103 C107 121.2(5) . . ? C105 C104 C103 123.3(5) . . ? C105 C104 H10B 118.4 . . ? C103 C104 H10B 118.4 . . ? C104 C105 C100 120.0(4) . . ? C104 C105 C108 116.6(4) . . ? C100 C105 C108 123.4(4) . . ? C101 C106 H10C 109.5 . . ? C101 C106 H10D 109.5 . . ? H10C C106 H10D 109.5 . . ? C101 C106 H10E 109.5 . . ? H10C C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C103 C107 H10F 109.5 . . ? C103 C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C103 C107 H10H 109.5 . . ? H10F C107 H10H 109.5 . . ? H10G C107 H10H 109.5 . . ? C105 C108 H10I 109.5 . . ? C105 C108 H10J 109.5 . . ? H10I C108 H10J 109.5 . . ? C105 C108 H10K 109.5 . . ? H10I C108 H10K 109.5 . . ? H10J C108 H10K 109.5 . . ? C201 C200 C205 117.7(4) . . ? C201 C200 Si4 125.5(3) . . ? C205 C200 Si4 116.8(3) . . ? C202 C201 C200 120.2(4) . . ? C202 C201 C206 116.7(4) . . ? C200 C201 C206 123.1(4) . . ? C203 C202 C201 122.3(4) . . ? C203 C202 H20B 118.8 . . ? C201 C202 H20B 118.8 . . ? C202 C203 C204 117.4(4) . . ? C202 C203 C207 121.8(5) . . ? C204 C203 C207 120.7(4) . . ? C205 C204 C203 122.5(4) . . ? C205 C204 H20C 118.7 . . ? C203 C204 H20C 118.7 . . ? C204 C205 C200 119.8(4) . . ? C204 C205 C208 118.4(4) . . ? C200 C205 C208 121.8(4) . . ? C201 C206 H20D 109.5 . . ? C201 C206 H20E 109.5 . . ? H20D C206 H20E 109.5 . . ? C201 C206 H20F 109.5 . . ? H20D C206 H20F 109.5 . . ? H20E C206 H20F 109.5 . . ? C203 C207 H20G 109.5 . . ? C203 C207 H20H 109.5 . . ? H20G C207 H20H 109.5 . . ? C203 C207 H20I 109.5 . . ? H20G C207 H20I 109.5 . . ? H20H C207 H20I 109.5 . . ? C205 C208 H20J 109.5 . . ? C205 C208 H20K 109.5 . . ? H20J C208 H20K 109.5 . . ? C205 C208 H20L 109.5 . . ? H20J C208 H20L 109.5 . . ? H20K C208 H20L 109.5 . . ? C301 C300 C305 117.8(3) . . ? C301 C300 Si1 117.7(3) . . ? C305 C300 Si1 124.4(3) . . ? C302 C301 C300 120.9(4) . . ? C302 C301 C306 117.0(4) . . ? C300 C301 C306 122.1(4) . . ? C303 C302 C301 121.2(4) . . ? C303 C302 H30A 119.4 . . ? C301 C302 H30A 119.4 . . ? C304 C303 C302 117.7(4) . . ? C304 C303 C307 121.3(4) . . ? C302 C303 C307 121.0(4) . . ? C303 C304 C305 123.5(4) . . ? C303 C304 H30B 118.2 . . ? C305 C304 H30B 118.2 . . ? C304 C305 C300 118.8(4) . . ? C304 C305 C308 117.0(4) . . ? C300 C305 C308 124.1(3) . . ? C301 C306 H30C 109.5 . . ? C301 C306 H30D 109.5 . . ? H30C C306 H30D 109.5 . . ? C301 C306 H30E 109.5 . . ? H30C C306 H30E 109.5 . . ? H30D C306 H30E 109.5 . . ? C303 C307 H30F 109.5 . . ? C303 C307 H30G 109.5 . . ? H30F C307 H30G 109.5 . . ? C303 C307 H30H 109.5 . . ? H30F C307 H30H 109.5 . . ? H30G C307 H30H 109.5 . . ? C305 C308 H30I 109.5 . . ? C305 C308 H30J 109.5 . . ? H30I C308 H30J 109.5 . . ? C305 C308 H30K 109.5 . . ? H30I C308 H30K 109.5 . . ? H30J C308 H30K 109.5 . . ? C94 C93 C98 120.2(7) . . ? C94 C93 H93A 119.9 . . ? C98 C93 H93A 119.9 . . ? C93 C94 C95 122.2(8) . . ? C93 C94 H94A 118.9 . . ? C95 C94 H94A 118.9 . . ? C96 C95 C94 118.1(9) . . ? C96 C95 H95A 120.9 . . ? C94 C95 H95A 120.9 . . ? C95 C96 C97 122.0(8) . . ? C95 C96 H96A 119.0 . . ? C97 C96 H96A 119.0 . . ? C98 C97 C96 120.9(8) . . ? C98 C97 H97A 119.6 . . ? C96 C97 H97A 119.6 . . ? C97 C98 C93 116.5(8) . . ? C97 C98 C99 122.8(9) . . ? C93 C98 C99 120.7(9) . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Sn1 Si1 C300 60.14(14) . . . 2_655 ? Si4 Sn1 Si1 C300 -69.22(14) 2_655 . . 2_655 ? Si4 Sn1 Si1 C300 -157.52(14) . . . 2_655 ? Sn1 Sn1 Si1 C300 -113.52(13) 2_655 . . 2_655 ? S2 Sn1 Si1 C300 -75.70(14) . . . . ? Si4 Sn1 Si1 C300 154.93(14) 2_655 . . . ? Si4 Sn1 Si1 C300 66.64(14) . . . . ? Sn1 Sn1 Si1 C300 110.64(14) 2_655 . . . ? S2 Sn1 Si1 Sn1 173.66(4) . . . 2_655 ? Si4 Sn1 Si1 Sn1 44.30(3) 2_655 . . 2_655 ? Si4 Sn1 Si1 Sn1 -44.00(3) . . . 2_655 ? Si1 Sn1 S2 C10 152.41(17) . . . . ? Si4 Sn1 S2 C10 -98.02(18) 2_655 . . . ? Si4 Sn1 S2 C10 32.93(19) . . . . ? S2 Sn1 Si4 C100 -76.14(15) . . . . ? Si1 Sn1 Si4 C100 153.82(14) . . . . ? Si4 Sn1 Si4 C100 65.56(14) 2_655 . . . ? Sn1 Sn1 Si4 C100 109.84(15) 2_655 . . . ? S2 Sn1 Si4 C200 59.46(16) . . . . ? Si1 Sn1 Si4 C200 -70.58(14) . . . . ? Si4 Sn1 Si4 C200 -158.83(14) 2_655 . . . ? Sn1 Sn1 Si4 C200 -114.55(15) 2_655 . . . ? S2 Sn1 Si4 Sn1 174.01(4) . . . 2_655 ? Si1 Sn1 Si4 Sn1 43.97(2) . . . 2_655 ? Si4 Sn1 Si4 Sn1 -44.28(4) 2_655 . . 2_655 ? Sn1 S2 C10 C11 -93.0(4) . . . . ? Sn1 S2 C10 C14 93.5(4) . . . . ? Sn1 S2 C10 Fe2 -179.7(2) . . . . ? C21 Fe2 C10 C11 -55.1(5) . . . . ? C20 Fe2 C10 C11 -92.5(4) . . . . ? C12 Fe2 C10 C11 37.2(5) . . . . ? C14 Fe2 C10 C11 120.5(5) . . . . ? C24 Fe2 C10 C11 -135.8(4) . . . . ? C13 Fe2 C10 C11 80.0(5) . . . . ? C23 Fe2 C10 C11 -173.9(4) . . . . ? C21 Fe2 C10 C14 -175.6(4) . . . . ? C20 Fe2 C10 C14 147.0(4) . . . . ? C12 Fe2 C10 C14 -83.2(5) . . . . ? C11 Fe2 C10 C14 -120.5(5) . . . . ? C24 Fe2 C10 C14 103.7(4) . . . . ? C13 Fe2 C10 C14 -40.4(5) . . . . ? C23 Fe2 C10 C14 65.6(5) . . . . ? C21 Fe2 C10 S2 64.2(5) . . . . ? C20 Fe2 C10 S2 26.9(4) . . . . ? C12 Fe2 C10 S2 156.6(5) . . . . ? C14 Fe2 C10 S2 -120.1(5) . . . . ? C11 Fe2 C10 S2 119.4(5) . . . . ? C24 Fe2 C10 S2 -16.5(4) . . . . ? C13 Fe2 C10 S2 -160.6(5) . . . . ? C23 Fe2 C10 S2 -54.5(4) . . . . ? C14 C10 C11 C12 -0.8(6) . . . . ? S2 C10 C11 C12 -175.3(4) . . . . ? Fe2 C10 C11 C12 -59.3(4) . . . . ? C14 C10 C11 Fe2 58.5(3) . . . . ? S2 C10 C11 Fe2 -116.0(3) . . . . ? C21 Fe2 C11 C12 -92.9(5) . . . . ? C20 Fe2 C11 C12 -137.0(5) . . . . ? C14 Fe2 C11 C12 82.1(5) . . . . ? C10 Fe2 C11 C12 119.2(6) . . . . ? C24 Fe2 C11 C12 -174.4(5) . . . . ? C22 Fe2 C11 C12 -58.7(7) . . . . ? C13 Fe2 C11 C12 36.8(5) . . . . ? C21 Fe2 C11 C10 147.8(3) . . . . ? C20 Fe2 C11 C10 103.7(3) . . . . ? C12 Fe2 C11 C10 -119.2(6) . . . . ? C14 Fe2 C11 C10 -37.1(3) . . . . ? C24 Fe2 C11 C10 66.4(5) . . . . ? C22 Fe2 C11 C10 -177.9(3) . . . . ? C13 Fe2 C11 C10 -82.5(4) . . . . ? C10 C11 C12 C13 -1.2(7) . . . . ? Fe2 C11 C12 C13 -60.4(5) . . . . ? C10 C11 C12 Fe2 59.2(4) . . . . ? C21 Fe2 C12 C13 -137.2(4) . . . . ? C20 Fe2 C12 C13 -176.7(4) . . . . ? C14 Fe2 C12 C13 38.0(4) . . . . ? C10 Fe2 C12 C13 82.0(4) . . . . ? C11 Fe2 C12 C13 119.9(6) . . . . ? C22 Fe2 C12 C13 -94.4(4) . . . . ? C23 Fe2 C12 C13 -59.0(7) . . . . ? C21 Fe2 C12 C11 102.9(4) . . . . ? C20 Fe2 C12 C11 63.4(5) . . . . ? C14 Fe2 C12 C11 -81.9(4) . . . . ? C10 Fe2 C12 C11 -37.9(4) . . . . ? C22 Fe2 C12 C11 145.7(4) . . . . ? C13 Fe2 C12 C11 -119.9(6) . . . . ? C23 Fe2 C12 C11 -178.9(4) . . . . ? C11 C12 C13 C14 2.6(8) . . . . ? Fe2 C12 C13 C14 -57.4(5) . . . . ? C11 C12 C13 Fe2 60.1(5) . . . . ? C21 Fe2 C13 C12 62.9(6) . . . . ? C14 Fe2 C13 C12 -120.7(6) . . . . ? C10 Fe2 C13 C12 -81.3(4) . . . . ? C11 Fe2 C13 C12 -37.2(4) . . . . ? C24 Fe2 C13 C12 -175.2(4) . . . . ? C22 Fe2 C13 C12 102.8(5) . . . . ? C23 Fe2 C13 C12 146.9(4) . . . . ? C21 Fe2 C13 C14 -176.5(4) . . . . ? C12 Fe2 C13 C14 120.7(6) . . . . ? C10 Fe2 C13 C14 39.3(4) . . . . ? C11 Fe2 C13 C14 83.5(4) . . . . ? C24 Fe2 C13 C14 -54.5(6) . . . . ? C22 Fe2 C13 C14 -136.5(4) . . . . ? C23 Fe2 C13 C14 -92.4(4) . . . . ? C11 C10 C14 C13 2.3(5) . . . . ? S2 C10 C14 C13 176.7(4) . . . . ? Fe2 C10 C14 C13 61.0(4) . . . . ? C11 C10 C14 Fe2 -58.7(3) . . . . ? S2 C10 C14 Fe2 115.8(3) . . . . ? C12 C13 C14 C10 -3.0(7) . . . . ? Fe2 C13 C14 C10 -61.1(4) . . . . ? C12 C13 C14 Fe2 58.1(5) . . . . ? C20 Fe2 C14 C10 -56.8(5) . . . . ? C12 Fe2 C14 C10 79.9(4) . . . . ? C11 Fe2 C14 C10 37.0(3) . . . . ? C24 Fe2 C14 C10 -93.6(4) . . . . ? C22 Fe2 C14 C10 -176.3(3) . . . . ? C13 Fe2 C14 C10 115.8(6) . . . . ? C23 Fe2 C14 C10 -137.4(3) . . . . ? C20 Fe2 C14 C13 -172.6(5) . . . . ? C12 Fe2 C14 C13 -35.9(5) . . . . ? C10 Fe2 C14 C13 -115.8(6) . . . . ? C11 Fe2 C14 C13 -78.8(5) . . . . ? C24 Fe2 C14 C13 150.6(5) . . . . ? C22 Fe2 C14 C13 67.9(6) . . . . ? C23 Fe2 C14 C13 106.8(5) . . . . ? C21 Fe2 C20 C24 119.0(5) . . . . ? C12 Fe2 C20 C24 -175.3(4) . . . . ? C14 Fe2 C20 C24 -58.0(5) . . . . ? C10 Fe2 C20 C24 -94.5(3) . . . . ? C11 Fe2 C20 C24 -138.0(3) . . . . ? C22 Fe2 C20 C24 81.5(3) . . . . ? C23 Fe2 C20 C24 37.7(3) . . . . ? C12 Fe2 C20 C21 65.7(5) . . . . ? C14 Fe2 C20 C21 -177.0(4) . . . . ? C10 Fe2 C20 C21 146.6(3) . . . . ? C11 Fe2 C20 C21 103.1(3) . . . . ? C24 Fe2 C20 C21 -119.0(5) . . . . ? C22 Fe2 C20 C21 -37.5(3) . . . . ? C23 Fe2 C20 C21 -81.3(3) . . . . ? C24 C20 C21 C22 0.4(6) . . . . ? Fe2 C20 C21 C22 60.8(3) . . . . ? C24 C20 C21 Fe2 -60.4(4) . . . . ? C20 Fe2 C21 C22 -118.6(5) . . . . ? C12 Fe2 C21 C22 105.5(4) . . . . ? C10 Fe2 C21 C22 -176.4(3) . . . . ? C11 Fe2 C21 C22 148.2(3) . . . . ? C24 Fe2 C21 C22 -81.1(4) . . . . ? C13 Fe2 C21 C22 68.7(6) . . . . ? C23 Fe2 C21 C22 -37.4(3) . . . . ? C12 Fe2 C21 C20 -136.0(4) . . . . ? C10 Fe2 C21 C20 -57.8(5) . . . . ? C11 Fe2 C21 C20 -93.2(4) . . . . ? C24 Fe2 C21 C20 37.4(3) . . . . ? C22 Fe2 C21 C20 118.6(5) . . . . ? C13 Fe2 C21 C20 -172.8(5) . . . . ? C23 Fe2 C21 C20 81.1(3) . . . . ? C20 C21 C22 C23 -0.7(6) . . . . ? Fe2 C21 C22 C23 59.1(4) . . . . ? C20 C21 C22 Fe2 -59.8(3) . . . . ? C20 Fe2 C22 C21 38.7(3) . . . . ? C12 Fe2 C22 C21 -90.9(5) . . . . ? C14 Fe2 C22 C21 -175.5(4) . . . . ? C11 Fe2 C22 C21 -53.9(6) . . . . ? C24 Fe2 C22 C21 82.2(4) . . . . ? C13 Fe2 C22 C21 -133.9(5) . . . . ? C23 Fe2 C22 C21 119.7(5) . . . . ? C21 Fe2 C22 C23 -119.7(5) . . . . ? C20 Fe2 C22 C23 -81.1(4) . . . . ? C12 Fe2 C22 C23 149.3(5) . . . . ? C14 Fe2 C22 C23 64.8(5) . . . . ? C11 Fe2 C22 C23 -173.7(4) . . . . ? C24 Fe2 C22 C23 -37.5(3) . . . . ? C13 Fe2 C22 C23 106.4(5) . . . . ? C21 C22 C23 C24 0.7(6) . . . . ? Fe2 C22 C23 C24 59.3(4) . . . . ? C21 C22 C23 Fe2 -58.6(3) . . . . ? C21 Fe2 C23 C24 -82.3(4) . . . . ? C20 Fe2 C23 C24 -37.5(3) . . . . ? C12 Fe2 C23 C24 -174.0(6) . . . . ? C14 Fe2 C23 C24 102.8(4) . . . . ? C10 Fe2 C23 C24 63.2(4) . . . . ? C22 Fe2 C23 C24 -119.3(5) . . . . ? C13 Fe2 C23 C24 148.5(4) . . . . ? C21 Fe2 C23 C22 37.1(3) . . . . ? C20 Fe2 C23 C22 81.8(3) . . . . ? C12 Fe2 C23 C22 -54.6(7) . . . . ? C14 Fe2 C23 C22 -137.9(3) . . . . ? C10 Fe2 C23 C22 -177.5(3) . . . . ? C24 Fe2 C23 C22 119.3(5) . . . . ? C13 Fe2 C23 C22 -92.2(4) . . . . ? C21 C20 C24 C23 0.0(6) . . . . ? Fe2 C20 C24 C23 -59.4(4) . . . . ? C21 C20 C24 Fe2 59.5(3) . . . . ? C22 C23 C24 C20 -0.5(6) . . . . ? Fe2 C23 C24 C20 58.8(4) . . . . ? C22 C23 C24 Fe2 -59.3(4) . . . . ? C21 Fe2 C24 C20 -38.4(3) . . . . ? C14 Fe2 C24 C20 146.2(3) . . . . ? C10 Fe2 C24 C20 102.2(3) . . . . ? C11 Fe2 C24 C20 62.6(4) . . . . ? C22 Fe2 C24 C20 -81.6(3) . . . . ? C13 Fe2 C24 C20 -177.2(4) . . . . ? C23 Fe2 C24 C20 -119.1(5) . . . . ? C21 Fe2 C24 C23 80.8(4) . . . . ? C20 Fe2 C24 C23 119.1(5) . . . . ? C14 Fe2 C24 C23 -94.6(4) . . . . ? C10 Fe2 C24 C23 -138.7(3) . . . . ? C11 Fe2 C24 C23 -178.2(3) . . . . ? C22 Fe2 C24 C23 37.6(3) . . . . ? C13 Fe2 C24 C23 -58.1(5) . . . . ? C200 Si4 C100 C101 66.3(4) . . . . ? Sn1 Si4 C100 C101 -72.2(3) 2_655 . . . ? Sn1 Si4 C100 C101 -156.1(3) . . . . ? C200 Si4 C100 C105 -114.3(4) . . . . ? Sn1 Si4 C100 C105 107.2(3) 2_655 . . . ? Sn1 Si4 C100 C105 23.3(4) . . . . ? C105 C100 C101 C102 0.1(6) . . . . ? Si4 C100 C101 C102 179.5(4) . . . . ? C105 C100 C101 C106 -179.2(4) . . . . ? Si4 C100 C101 C106 0.2(6) . . . . ? C100 C101 C102 C103 -0.7(8) . . . . ? C106 C101 C102 C103 178.6(5) . . . . ? C101 C102 C103 C104 0.2(9) . . . . ? C101 C102 C103 C107 -178.9(6) . . . . ? C102 C103 C104 C105 0.9(8) . . . . ? C107 C103 C104 C105 -180.0(6) . . . . ? C103 C104 C105 C100 -1.5(8) . . . . ? C103 C104 C105 C108 179.4(5) . . . . ? C101 C100 C105 C104 1.0(6) . . . . ? Si4 C100 C105 C104 -178.4(4) . . . . ? C101 C100 C105 C108 180.0(4) . . . . ? Si4 C100 C105 C108 0.6(6) . . . . ? C100 Si4 C200 C201 -111.6(4) . . . . ? Sn1 Si4 C200 C201 25.2(4) 2_655 . . . ? Sn1 Si4 C200 C201 109.1(3) . . . . ? C100 Si4 C200 C205 66.8(4) . . . . ? Sn1 Si4 C200 C205 -156.4(3) 2_655 . . . ? Sn1 Si4 C200 C205 -72.5(3) . . . . ? C205 C200 C201 C202 -0.4(6) . . . . ? Si4 C200 C201 C202 178.1(3) . . . . ? C205 C200 C201 C206 177.4(4) . . . . ? Si4 C200 C201 C206 -4.2(6) . . . . ? C200 C201 C202 C203 1.4(6) . . . . ? C206 C201 C202 C203 -176.5(4) . . . . ? C201 C202 C203 C204 -0.6(7) . . . . ? C201 C202 C203 C207 179.2(4) . . . . ? C202 C203 C204 C205 -1.2(7) . . . . ? C207 C203 C204 C205 179.0(4) . . . . ? C203 C204 C205 C200 2.2(7) . . . . ? C203 C204 C205 C208 -179.4(4) . . . . ? C201 C200 C205 C204 -1.4(6) . . . . ? Si4 C200 C205 C204 -180.0(3) . . . . ? C201 C200 C205 C208 -179.7(4) . . . . ? Si4 C200 C205 C208 1.8(5) . . . . ? C300 Si1 C300 C301 63.0(3) 2_655 . . . ? Sn1 Si1 C300 C301 -75.5(3) 2_655 . . . ? Sn1 Si1 C300 C301 -159.6(3) . . . . ? C300 Si1 C300 C305 -119.3(4) 2_655 . . . ? Sn1 Si1 C300 C305 102.2(3) 2_655 . . . ? Sn1 Si1 C300 C305 18.1(4) . . . . ? C305 C300 C301 C302 0.2(6) . . . . ? Si1 C300 C301 C302 178.0(3) . . . . ? C305 C300 C301 C306 -178.2(4) . . . . ? Si1 C300 C301 C306 -0.4(5) . . . . ? C300 C301 C302 C303 -1.0(6) . . . . ? C306 C301 C302 C303 177.5(4) . . . . ? C301 C302 C303 C304 0.4(6) . . . . ? C301 C302 C303 C307 179.7(4) . . . . ? C302 C303 C304 C305 1.2(6) . . . . ? C307 C303 C304 C305 -178.1(4) . . . . ? C303 C304 C305 C300 -2.0(6) . . . . ? C303 C304 C305 C308 175.7(4) . . . . ? C301 C300 C305 C304 1.3(6) . . . . ? Si1 C300 C305 C304 -176.4(3) . . . . ? C301 C300 C305 C308 -176.3(4) . . . . ? Si1 C300 C305 C308 6.0(6) . . . . ? C98 C93 C94 C95 -1.8(15) . . . . ? C93 C94 C95 C96 0.2(15) . . . . ? C94 C95 C96 C97 2.6(13) . . . . ? C95 C96 C97 C98 -3.9(12) . . . . ? C96 C97 C98 C93 2.2(11) . . . . ? C96 C97 C98 C99 -179.2(7) . . . . ? C94 C93 C98 C97 0.6(12) . . . . ? C94 C93 C98 C99 -178.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.380 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.099