#------------------------------------------------------------------------------ #$Date: 2021-09-30 03:44:12 +0300 (Thu, 30 Sep 2021) $ #$Revision: 269387 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060974.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7060974 loop_ _publ_author_name 'Loganathan, Pushparaj' 'Pillai, Renjith S.' 'Jeevananthan, Velusamy' 'David, Ezhumalai' 'Palanisami, Nallasamy' 'Bhuvanesh, Nattamai' 'Shanmugan, Swaminathan' _publ_section_title ; Assembly of Discrete and Oligomeric Structures of Organotin Double-decker Silsesquioxanes: Inherent Stability Studies ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ03128G _journal_year 2021 _chemical_formula_moiety 'C32 H38 O7 Si4 Sn' _chemical_formula_sum 'C32 H38 O7 Si4 Sn' _chemical_formula_weight 765.67 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-09-25 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _cell_angle_alpha 115.770(7) _cell_angle_beta 102.852(7) _cell_angle_gamma 101.735(5) _cell_formula_units_Z 2 _cell_length_a 11.0582(12) _cell_length_b 13.6018(11) _cell_length_c 14.649(2) _cell_measurement_reflns_used 4224 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 56.147 _cell_measurement_theta_min 5.240 _cell_volume 1818.0(4) _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altornare et al., 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_unetI/netI 0.0626 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11597 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 24.997 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_min 2.103 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_correction_T_min 0.621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.399 _exptl_crystal_description block _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 1.180 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 400 _refine_ls_number_reflns 6322 _refine_ls_number_restraints 184 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0460 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1188 _refine_ls_wR_factor_ref 0.1430 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4914 _reflns_number_total 6322 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj03128g2.cif _cod_data_source_block shelx _cod_database_code 7060974 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.621 _shelx_estimated_absorpt_t_max 0.844 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 0.71073 11.0582 13.6018 14.6492 115.770 102.852 101.735 ZERR 2.00 0.0012 0.0011 0.0021 0.007 0.007 0.005 LATT 1 SFAC C H O SI SN UNIT 64 76 14 8 2 MERG 2 OMIT -3.00 50.00 OMIT 1 -1 1 OMIT -1 -1 1 OMIT 0 0 1 OMIT 0 1 0 OMIT 1 0 0 OMIT -8 -1 3 OMIT 7 0 5 DFIX 1.54 0.02 C31 C32 DELU 0.01 C30 C31 DELU 0.01 C31 C32 DELU 0.01 C27 C28 SIMU 0.04 $C FMAP 2 PLAN 5 SIZE 0.200 0.300 0.600 ACTA BOND $H L.S. 30 TEMP 23.00 WGHT 0.087600 FVAR 0.15074 0.51435 C29 1 0.003684 0.514266 0.307517 11.00000 0.05845 0.11495 = 0.09247 0.08105 0.03659 0.04427 AFIX 23 H29A 2 -0.053378 0.460789 0.232701 11.00000 -1.20000 H29B 2 -0.044482 0.561819 0.342778 11.00000 -1.20000 AFIX 0 C1 1 0.328596 0.316988 0.727501 11.00000 0.07302 0.10567 = 0.09771 0.07639 0.03795 0.02431 AFIX 43 H1 2 0.255188 0.289427 0.666214 11.00000 -1.20000 AFIX 0 C2 1 0.318343 0.282467 0.802969 11.00000 0.11060 0.11986 = 0.13889 0.09537 0.06423 0.03666 AFIX 43 H2 2 0.237781 0.233249 0.791696 11.00000 -1.20000 AFIX 0 C3 1 0.421646 0.318572 0.890926 11.00000 0.17124 0.10989 = 0.09813 0.07867 0.07573 0.05543 AFIX 43 H3 2 0.414123 0.293349 0.939769 11.00000 -1.20000 AFIX 0 C4 1 0.535429 0.391016 0.907899 11.00000 0.17621 0.10324 = 0.06438 0.05841 0.01551 0.04249 AFIX 43 H4 2 0.606963 0.418067 0.970342 11.00000 -1.20000 AFIX 0 C5 1 0.550438 0.427497 0.834763 11.00000 0.09233 0.07132 = 0.05670 0.03876 0.01116 0.02319 AFIX 43 H5 2 0.631814 0.476988 0.847783 11.00000 -1.20000 AFIX 0 C6 1 0.443637 0.389992 0.741870 11.00000 0.06118 0.04638 = 0.04654 0.02787 0.03045 0.03334 C7 1 0.316563 0.663822 0.833389 11.00000 0.07272 0.07657 = 0.04644 0.02828 0.01962 0.03453 AFIX 43 H7 2 0.304017 0.587485 0.817011 11.00000 -1.20000 AFIX 0 C8 1 0.329645 0.746689 0.936479 11.00000 0.10265 0.11520 = 0.04653 0.03299 0.02415 0.04524 AFIX 43 H8 2 0.324387 0.725196 0.988074 11.00000 -1.20000 AFIX 0 C9 1 0.349926 0.858134 0.962175 11.00000 0.08418 0.08671 = 0.05660 0.00611 0.02355 0.02506 AFIX 43 H9 2 0.357547 0.912703 1.031219 11.00000 -1.20000 AFIX 0 C10 1 0.359427 0.891899 0.887947 11.00000 0.07676 0.05833 = 0.06749 0.00710 0.01987 0.02363 AFIX 43 H10 2 0.374194 0.968971 0.906114 11.00000 -1.20000 AFIX 0 C11 1 0.346636 0.809089 0.785020 11.00000 0.04439 0.04739 = 0.05161 0.00955 0.01446 0.01035 AFIX 43 H11 2 0.354919 0.832140 0.734872 11.00000 -1.20000 AFIX 0 C12 1 0.321938 0.693268 0.754642 11.00000 0.02747 0.05571 = 0.03618 0.01469 0.00595 0.01695 C13 1 0.476430 0.128565 0.378992 11.00000 0.05419 0.03815 = 0.05678 0.02423 0.03190 0.02448 C14 1 0.376559 0.035594 0.291103 11.00000 0.11420 0.03264 = 0.06333 0.01316 0.01463 0.01589 AFIX 43 H14 2 0.307191 0.047489 0.252984 11.00000 -1.20000 AFIX 0 C15 1 0.377329 -0.077879 0.257546 11.00000 0.19501 0.03917 = 0.08402 0.01316 0.04053 0.02688 AFIX 43 H15 2 0.311451 -0.140034 0.194915 11.00000 -1.20000 AFIX 0 C30 1 0.117008 0.588032 0.308971 11.00000 0.12284 0.21962 = 0.28344 0.21778 0.09452 0.07529 AFIX 23 H30A 2 0.161994 0.539848 0.269629 11.00000 -1.20000 H30B 2 0.176716 0.637993 0.383473 11.00000 -1.20000 AFIX 0 C16 1 0.469734 -0.096741 0.313556 11.00000 0.17610 0.05297 = 0.15223 0.04979 0.08300 0.06318 AFIX 43 H16 2 0.465300 -0.172643 0.293720 11.00000 -1.20000 AFIX 0 C17 1 0.568373 -0.010354 0.397128 11.00000 0.13366 0.08282 = 0.21373 0.08116 0.03093 0.05952 AFIX 43 H17 2 0.636110 -0.025072 0.433773 11.00000 -1.20000 AFIX 0 C18 1 0.572979 0.105104 0.432249 11.00000 0.09373 0.05946 = 0.16785 0.05777 -0.00906 0.03448 AFIX 43 H18 2 0.643068 0.165837 0.492645 11.00000 -1.20000 AFIX 0 C19 1 0.194730 0.245944 0.141824 11.00000 0.05406 0.04275 = 0.02948 0.01253 0.00650 0.01590 C20 1 0.255946 0.197151 0.069333 11.00000 0.08828 0.12075 = 0.06259 0.01247 0.02260 0.04556 AFIX 43 H20 2 0.346938 0.215031 0.094415 11.00000 -1.20000 AFIX 0 C21 1 0.183599 0.121717 -0.040558 11.00000 0.14209 0.14418 = 0.05312 -0.00251 0.01644 0.07209 AFIX 43 H21 2 0.224966 0.088255 -0.088813 11.00000 -1.20000 AFIX 0 C22 1 0.047753 0.097715 -0.076278 11.00000 0.12486 0.15941 = 0.04078 -0.00333 -0.01533 0.03393 AFIX 43 H22 2 -0.002346 0.046462 -0.149133 11.00000 -1.20000 AFIX 0 C23 1 -0.010580 0.146193 -0.008875 11.00000 0.08821 0.22438 = 0.06344 -0.01777 -0.01909 0.05922 AFIX 43 H23 2 -0.100703 0.132460 -0.034011 11.00000 -1.20000 AFIX 0 C24 1 0.062694 0.217185 0.098824 11.00000 0.06841 0.18282 = 0.05739 0.00544 0.01115 0.05065 AFIX 43 H24 2 0.018698 0.247809 0.145744 11.00000 -1.20000 AFIX 0 C25 1 -0.036531 0.253808 0.370340 11.00000 0.04426 0.04739 = 0.09992 0.03071 0.02807 0.01552 AFIX 23 H25A 2 -0.088656 0.262535 0.416766 11.00000 -1.20000 H25B 2 -0.095899 0.199472 0.296388 11.00000 -1.20000 AFIX 0 C26 1 0.061683 0.202364 0.399226 11.00000 0.07188 0.08207 = 0.16167 0.08137 0.03770 0.03123 AFIX 23 H26A 2 0.126206 0.258845 0.470704 11.00000 -1.20000 H26B 2 0.107868 0.185504 0.348186 11.00000 -1.20000 AFIX 0 C27 1 -0.000835 0.090957 0.398741 11.00000 0.12884 0.09149 = 0.15275 0.08507 0.06605 0.05412 AFIX 23 H27A 2 -0.071921 0.037254 0.329956 11.00000 -1.20000 H27B 2 -0.038280 0.109070 0.455535 11.00000 -1.20000 AFIX 0 C28 1 0.098903 0.033887 0.416103 11.00000 0.23940 0.18611 = 0.24274 0.15619 0.11844 0.13613 AFIX 137 H28A 2 0.137522 0.017411 0.360897 11.00000 -1.50000 H28B 2 0.055863 -0.037211 0.412490 11.00000 -1.50000 H28C 2 0.166751 0.085167 0.485961 11.00000 -1.50000 AFIX 0 O1 3 0.368006 0.277507 0.332429 11.00000 0.03721 0.04498 = 0.05006 0.02130 0.01003 0.01843 O2 3 0.623727 0.355049 0.436483 11.00000 0.03056 0.03602 = 0.04835 0.01979 0.01554 0.00956 O3 3 0.464256 0.335976 0.538648 11.00000 0.04713 0.04026 = 0.04713 0.02156 0.02345 0.01989 O4 3 0.594707 0.548576 0.703443 11.00000 0.03612 0.04489 = 0.04939 0.02144 0.01201 0.00914 O5 3 0.336906 0.476446 0.612146 11.00000 0.03473 0.04145 = 0.05201 0.02508 0.01271 0.01963 O6 3 0.138185 0.533869 0.542925 11.00000 0.02305 0.03976 = 0.03870 0.01657 0.00959 0.01199 O7 3 0.206855 0.397101 0.354868 11.00000 0.03732 0.06041 = 0.05183 0.01943 0.02299 0.02620 SI1 4 0.461864 0.439881 0.645892 11.00000 0.03094 0.03150 = 0.03733 0.01908 0.01253 0.01332 SI2 4 0.482445 0.279466 0.423027 11.00000 0.02992 0.02682 = 0.03817 0.01539 0.01115 0.01127 SI3 4 0.292812 0.347152 0.287545 11.00000 0.02353 0.03408 = 0.03291 0.01230 0.00784 0.01046 SI4 4 0.292521 0.583033 0.612967 11.00000 0.02151 0.03491 = 0.03758 0.01636 0.01092 0.01297 SN1 5 0.042485 0.416277 0.383263 11.00000 0.02726 0.03948 = 0.03991 0.01706 0.01093 0.01450 C31 1 0.090282 0.665107 0.260496 11.00000 0.16195 0.25381 = 0.32755 0.25086 0.05938 0.03652 AFIX 23 H31A 2 0.045302 0.713418 0.299699 11.00000 -1.20000 H31B 2 0.174313 0.716300 0.272094 11.00000 -1.20000 AFIX 0 C32 1 0.014982 0.604949 0.150102 11.00000 0.37576 0.41735 = 0.33617 0.30068 0.01525 0.09756 AFIX 137 H32A 2 -0.029878 0.525544 0.127682 11.00000 -1.50000 H32B 2 0.071771 0.607632 0.109664 11.00000 -1.50000 H32C 2 -0.048696 0.640328 0.137094 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0460 for 4914 Fo > 4sig(Fo) and 0.0666 for all 6322 data REM 400 parameters refined using 184 restraints END WGHT 0.0743 0.0000 REM Highest difference peak 1.180, deepest hole -0.709, 1-sigma level 0.098 Q1 1 0.1411 0.4399 0.4126 11.00000 0.05 1.18 Q2 1 -0.0558 0.3991 0.3556 11.00000 0.05 0.73 Q3 1 0.0194 0.4392 0.3146 11.00000 0.05 0.68 Q4 1 0.0365 0.5244 0.2249 11.00000 0.05 0.60 Q5 1 0.3823 0.4449 0.6436 11.00000 0.05 0.56 ; _shelx_res_checksum 44362 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C29 C 0.0037(7) 0.5143(7) 0.3075(6) 0.072(2) Uani 1 1 d . U . . . H29A H -0.0534 0.4608 0.2327 0.087 Uiso 1 1 calc R U . . . H29B H -0.0445 0.5618 0.3428 0.087 Uiso 1 1 calc R U . . . C1 C 0.3286(8) 0.3170(7) 0.7275(6) 0.081(2) Uani 1 1 d . U . . . H1 H 0.2552 0.2894 0.6662 0.098 Uiso 1 1 calc R U . . . C2 C 0.3183(11) 0.2825(8) 0.8030(9) 0.107(3) Uani 1 1 d . U . . . H2 H 0.2378 0.2332 0.7917 0.129 Uiso 1 1 calc R U . . . C3 C 0.4216(13) 0.3186(9) 0.8909(8) 0.109(3) Uani 1 1 d . U . . . H3 H 0.4141 0.2933 0.9398 0.131 Uiso 1 1 calc R U . . . C4 C 0.5354(12) 0.3910(8) 0.9079(7) 0.114(4) Uani 1 1 d . U . . . H4 H 0.6070 0.4181 0.9703 0.137 Uiso 1 1 calc R U . . . C5 C 0.5504(8) 0.4275(6) 0.8348(5) 0.075(2) Uani 1 1 d . U . . . H5 H 0.6318 0.4770 0.8478 0.089 Uiso 1 1 calc R U . . . C6 C 0.4436(6) 0.3900(4) 0.7419(4) 0.0447(13) Uani 1 1 d . U . . . C7 C 0.3166(7) 0.6638(6) 0.8334(5) 0.0650(17) Uani 1 1 d . U . . . H7 H 0.3040 0.5875 0.8170 0.078 Uiso 1 1 calc R U . . . C8 C 0.3296(9) 0.7467(8) 0.9365(5) 0.090(2) Uani 1 1 d . U . . . H8 H 0.3244 0.7252 0.9881 0.108 Uiso 1 1 calc R U . . . C9 C 0.3499(8) 0.8581(7) 0.9622(6) 0.089(2) Uani 1 1 d . U . . . H9 H 0.3575 0.9127 1.0312 0.107 Uiso 1 1 calc R U . . . C10 C 0.3594(8) 0.8919(6) 0.8879(6) 0.078(2) Uani 1 1 d . U . . . H10 H 0.3742 0.9690 0.9061 0.094 Uiso 1 1 calc R U . . . C11 C 0.3466(6) 0.8091(5) 0.7850(5) 0.0554(15) Uani 1 1 d . U . . . H11 H 0.3549 0.8321 0.7349 0.067 Uiso 1 1 calc R U . . . C12 C 0.3219(5) 0.6933(5) 0.7546(4) 0.0437(12) Uani 1 1 d . U . . . C13 C 0.4764(6) 0.1286(4) 0.3790(4) 0.0457(13) Uani 1 1 d . U . . . C14 C 0.3766(8) 0.0356(5) 0.2911(5) 0.079(2) Uani 1 1 d . U . . . H14 H 0.3072 0.0475 0.2530 0.095 Uiso 1 1 calc R U . . . C15 C 0.3773(13) -0.0779(6) 0.2575(7) 0.117(4) Uani 1 1 d . U . . . H15 H 0.3115 -0.1400 0.1949 0.141 Uiso 1 1 calc R U . . . C30 C 0.1170(11) 0.5880(11) 0.3090(12) 0.164(5) Uani 1 1 d . U . . . H30A H 0.1620 0.5398 0.2696 0.197 Uiso 1 1 calc R U . . . H30B H 0.1767 0.6380 0.3835 0.197 Uiso 1 1 calc R U . . . C16 C 0.4697(14) -0.0967(8) 0.3136(10) 0.119(4) Uani 1 1 d . U . . . H16 H 0.4653 -0.1726 0.2937 0.143 Uiso 1 1 calc R U . . . C17 C 0.5684(12) -0.0104(9) 0.3971(11) 0.143(4) Uani 1 1 d . U . . . H17 H 0.6361 -0.0251 0.4338 0.171 Uiso 1 1 calc R U . . . C18 C 0.5730(9) 0.1051(7) 0.4322(8) 0.116(4) Uani 1 1 d . U . . . H18 H 0.6431 0.1658 0.4926 0.139 Uiso 1 1 calc R U . . . C19 C 0.1947(6) 0.2459(4) 0.1418(4) 0.0461(13) Uani 1 1 d . U . . . C20 C 0.2559(10) 0.1972(8) 0.0693(6) 0.103(3) Uani 1 1 d . U . . . H20 H 0.3469 0.2150 0.0944 0.124 Uiso 1 1 calc R U . . . C21 C 0.1836(12) 0.1217(9) -0.0406(7) 0.134(4) Uani 1 1 d . U . . . H21 H 0.2250 0.0883 -0.0888 0.160 Uiso 1 1 calc R U . . . C22 C 0.0478(12) 0.0977(10) -0.0763(7) 0.141(4) Uani 1 1 d . U . . . H22 H -0.0023 0.0465 -0.1491 0.170 Uiso 1 1 calc R U . . . C23 C -0.0106(11) 0.1462(12) -0.0089(7) 0.170(6) Uani 1 1 d . U . . . H23 H -0.1007 0.1325 -0.0340 0.204 Uiso 1 1 calc R U . . . C24 C 0.0627(9) 0.2172(10) 0.0988(6) 0.126(4) Uani 1 1 d . U . . . H24 H 0.0187 0.2478 0.1457 0.151 Uiso 1 1 calc R U . . . C25 C -0.0365(6) 0.2538(5) 0.3703(6) 0.0659(18) Uani 1 1 d . U . . . H25A H -0.0887 0.2625 0.4168 0.079 Uiso 1 1 calc R U . . . H25B H -0.0959 0.1995 0.2964 0.079 Uiso 1 1 calc R U . . . C26 C 0.0617(8) 0.2024(7) 0.3992(8) 0.097(3) Uani 1 1 d . U . . . H26A H 0.1262 0.2588 0.4707 0.116 Uiso 1 1 calc R U . . . H26B H 0.1079 0.1855 0.3482 0.116 Uiso 1 1 calc R U . . . C27 C -0.0008(10) 0.0910(7) 0.3987(8) 0.109(3) Uani 1 1 d . U . . . H27A H -0.0719 0.0373 0.3300 0.130 Uiso 1 1 calc R U . . . H27B H -0.0383 0.1091 0.4555 0.130 Uiso 1 1 calc R U . . . C28 C 0.0989(14) 0.0339(12) 0.4161(11) 0.186(6) Uani 1 1 d . U . . . H28A H 0.1375 0.0174 0.3609 0.278 Uiso 1 1 calc R U . . . H28B H 0.0559 -0.0372 0.4125 0.278 Uiso 1 1 calc R U . . . H28C H 0.1668 0.0852 0.4860 0.278 Uiso 1 1 calc R U . . . O1 O 0.3680(4) 0.2775(3) 0.3324(3) 0.0454(9) Uani 1 1 d . . . . . O2 O 0.6237(3) 0.3550(3) 0.4365(3) 0.0389(8) Uani 1 1 d . . . . . O3 O 0.4643(4) 0.3360(3) 0.5386(3) 0.0428(8) Uani 1 1 d . . . . . O4 O 0.5947(4) 0.5486(3) 0.7034(3) 0.0458(9) Uani 1 1 d . . . . . O5 O 0.3369(3) 0.4764(3) 0.6121(3) 0.0414(8) Uani 1 1 d . . . . . O6 O 0.1382(3) 0.5339(3) 0.5429(2) 0.0352(7) Uani 1 1 d . . . . . O7 O 0.2069(4) 0.3971(3) 0.3549(3) 0.0504(9) Uani 1 1 d . . . . . Si1 Si 0.46186(13) 0.43988(11) 0.64589(10) 0.0320(3) Uani 1 1 d . . . . . Si2 Si 0.48244(13) 0.27947(10) 0.42303(10) 0.0319(3) Uani 1 1 d . . . . . Si3 Si 0.29281(13) 0.34715(11) 0.28755(10) 0.0323(3) Uani 1 1 d . . . . . Si4 Si 0.29252(12) 0.58303(11) 0.61297(10) 0.0314(3) Uani 1 1 d . . . . . Sn1 Sn 0.04248(3) 0.41628(3) 0.38326(3) 0.03636(14) Uani 1 1 d . . . . . C31 C 0.0903(15) 0.6651(13) 0.2605(14) 0.216(7) Uani 1 1 d D U . . . H31A H 0.0453 0.7134 0.2997 0.260 Uiso 1 1 calc R U . . . H31B H 0.1743 0.7163 0.2721 0.260 Uiso 1 1 calc R U . . . C32 C 0.015(2) 0.6049(18) 0.1501(15) 0.359(16) Uani 1 1 d D U . . . H32A H -0.0299 0.5255 0.1277 0.539 Uiso 1 1 calc R U . . . H32B H 0.0718 0.6076 0.1097 0.539 Uiso 1 1 calc R U . . . H32C H -0.0487 0.6403 0.1371 0.539 Uiso 1 1 calc R U . . . 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 C29 0.058(4) 0.115(6) 0.092(5) 0.081(5) 0.037(4) 0.044(4) C1 0.073(5) 0.106(5) 0.098(5) 0.076(5) 0.038(4) 0.024(4) C2 0.111(8) 0.120(7) 0.139(8) 0.095(7) 0.064(7) 0.037(6) C3 0.171(11) 0.110(7) 0.098(7) 0.079(6) 0.076(7) 0.055(7) C4 0.176(11) 0.103(6) 0.064(5) 0.058(5) 0.016(6) 0.042(7) C5 0.092(6) 0.071(4) 0.057(4) 0.039(3) 0.011(4) 0.023(4) C6 0.061(4) 0.046(3) 0.047(3) 0.028(2) 0.030(3) 0.033(3) C7 0.073(5) 0.077(4) 0.046(3) 0.028(3) 0.020(3) 0.035(4) C8 0.103(7) 0.115(7) 0.047(4) 0.033(4) 0.024(4) 0.045(5) C9 0.084(6) 0.087(5) 0.057(4) 0.006(4) 0.024(4) 0.025(5) C10 0.077(5) 0.058(4) 0.067(4) 0.007(3) 0.020(4) 0.024(4) C11 0.044(4) 0.047(3) 0.052(3) 0.010(3) 0.014(3) 0.010(3) C12 0.027(3) 0.056(3) 0.036(3) 0.015(2) 0.006(2) 0.017(2) C13 0.054(4) 0.038(3) 0.057(3) 0.024(3) 0.032(3) 0.024(3) C14 0.114(7) 0.033(3) 0.063(4) 0.013(3) 0.015(4) 0.016(4) C15 0.195(11) 0.039(4) 0.084(6) 0.013(4) 0.041(7) 0.027(5) C30 0.123(9) 0.220(11) 0.283(13) 0.218(11) 0.095(9) 0.075(8) C16 0.176(11) 0.053(5) 0.152(9) 0.050(6) 0.083(9) 0.063(6) C17 0.134(10) 0.083(6) 0.214(12) 0.081(7) 0.031(9) 0.060(6) C18 0.094(7) 0.059(4) 0.168(8) 0.058(5) -0.009(6) 0.034(4) C19 0.054(4) 0.043(3) 0.029(3) 0.013(2) 0.006(2) 0.016(3) C20 0.088(6) 0.121(7) 0.063(5) 0.012(4) 0.023(4) 0.046(5) C21 0.142(10) 0.144(8) 0.053(5) -0.003(5) 0.016(6) 0.072(8) C22 0.125(9) 0.159(9) 0.041(4) -0.003(5) -0.015(5) 0.034(8) C23 0.088(8) 0.224(12) 0.063(6) -0.018(7) -0.019(5) 0.059(8) C24 0.068(6) 0.183(9) 0.057(5) 0.005(5) 0.011(4) 0.051(6) C25 0.044(4) 0.047(3) 0.100(5) 0.031(3) 0.028(4) 0.016(3) C26 0.072(5) 0.082(5) 0.162(8) 0.081(6) 0.038(5) 0.031(4) C27 0.129(8) 0.091(6) 0.153(8) 0.085(6) 0.066(7) 0.054(6) C28 0.239(17) 0.186(12) 0.243(15) 0.156(12) 0.118(13) 0.136(12) O1 0.037(2) 0.045(2) 0.050(2) 0.0213(17) 0.0100(17) 0.0184(17) O2 0.0306(19) 0.0360(18) 0.048(2) 0.0198(16) 0.0155(16) 0.0096(15) O3 0.047(2) 0.0403(18) 0.047(2) 0.0216(16) 0.0234(18) 0.0199(17) O4 0.036(2) 0.045(2) 0.049(2) 0.0214(17) 0.0120(17) 0.0091(17) O5 0.035(2) 0.0415(19) 0.052(2) 0.0251(17) 0.0127(17) 0.0196(16) O6 0.0231(18) 0.0398(18) 0.0387(18) 0.0166(15) 0.0096(15) 0.0120(15) O7 0.037(2) 0.060(2) 0.052(2) 0.0194(18) 0.0230(18) 0.0262(19) Si1 0.0309(8) 0.0315(7) 0.0373(7) 0.0191(6) 0.0125(6) 0.0133(6) Si2 0.0299(7) 0.0268(6) 0.0382(7) 0.0154(5) 0.0111(6) 0.0113(5) Si3 0.0235(7) 0.0341(7) 0.0329(7) 0.0123(6) 0.0078(6) 0.0105(6) Si4 0.0215(7) 0.0349(7) 0.0376(7) 0.0164(6) 0.0109(6) 0.0130(6) Sn1 0.0273(2) 0.0395(2) 0.0399(2) 0.01706(16) 0.01093(15) 0.01450(15) C31 0.162(13) 0.254(15) 0.328(18) 0.251(15) 0.059(13) 0.037(11) C32 0.38(3) 0.42(3) 0.34(2) 0.30(2) 0.02(2) 0.10(2) 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' O O 0.0106 0.0060 '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' 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 C30 C29 Sn1 115.6(6) . . ? C30 C29 H29A 108.4 . . ? Sn1 C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? Sn1 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? C6 C1 C2 121.1(8) . . ? C6 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C3 C2 C1 121.3(9) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 119.1(8) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.7(9) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C4 C5 C6 120.1(8) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 116.8(6) . . ? C1 C6 Si1 122.9(5) . . ? C5 C6 Si1 120.3(5) . . ? C12 C7 C8 120.9(7) . . ? C12 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.4(7) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.8(7) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 118.8(7) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 122.1(6) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C7 117.0(5) . . ? C11 C12 Si4 120.8(4) . . ? C7 C12 Si4 122.2(4) . . ? C18 C13 C14 116.7(6) . . ? C18 C13 Si2 121.2(5) . . ? C14 C13 Si2 122.2(5) . . ? C13 C14 C15 120.7(8) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 120.5(9) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C29 C30 C31 115.9(10) . . ? C29 C30 H30A 108.3 . . ? C31 C30 H30A 108.3 . . ? C29 C30 H30B 108.3 . . ? C31 C30 H30B 108.3 . . ? H30A C30 H30B 107.4 . . ? C15 C16 C17 120.8(8) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 120.5(10) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.7(9) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C24 C19 C20 115.8(6) . . ? C24 C19 Si3 123.6(5) . . ? C20 C19 Si3 120.5(5) . . ? C19 C20 C21 121.1(9) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 118.3(9) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C23 C22 C21 121.0(8) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.1(10) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C19 C24 C23 124.5(9) . . ? C19 C24 H24 117.8 . . ? C23 C24 H24 117.8 . . ? C26 C25 Sn1 115.6(5) . . ? C26 C25 H25A 108.4 . . ? Sn1 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? Sn1 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C25 C26 C27 113.0(7) . . ? C25 C26 H26A 109.0 . . ? C27 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? C27 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C26 C27 C28 111.6(9) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 O1 Si3 149.6(2) . . ? Si2 O2 Si4 147.1(2) . 2_666 ? Si1 O3 Si2 154.7(2) . . ? Si1 O4 Si3 156.0(2) . 2_666 ? Si1 O5 Si4 144.1(2) . . ? Si4 O6 Sn1 129.18(19) . . ? Si4 O6 Sn1 125.64(17) . 2_566 ? Sn1 O6 Sn1 105.12(13) . 2_566 ? Si3 O7 Sn1 157.2(2) . . ? O4 Si1 O3 111.2(2) . . ? O4 Si1 O5 110.28(19) . . ? O3 Si1 O5 108.22(19) . . ? O4 Si1 C6 108.5(2) . . ? O3 Si1 C6 109.6(2) . . ? O5 Si1 C6 109.0(2) . . ? O1 Si2 O2 110.04(19) . . ? O1 Si2 O3 111.3(2) . . ? O2 Si2 O3 107.97(19) . . ? O1 Si2 C13 108.2(2) . . ? O2 Si2 C13 109.4(2) . . ? O3 Si2 C13 109.8(2) . . ? O7 Si3 O4 110.3(2) . 2_666 ? O7 Si3 O1 111.2(2) . . ? O4 Si3 O1 107.25(19) 2_666 . ? O7 Si3 C19 112.7(2) . . ? O4 Si3 C19 107.5(2) 2_666 . ? O1 Si3 C19 107.6(2) . . ? O6 Si4 O2 109.90(18) . 2_666 ? O6 Si4 O5 108.76(18) . . ? O2 Si4 O5 111.08(19) 2_666 . ? O6 Si4 C12 109.4(2) . . ? O2 Si4 C12 108.3(2) 2_666 . ? O5 Si4 C12 109.5(2) . . ? O7 Sn1 O6 94.18(14) . . ? O7 Sn1 C25 98.0(2) . . ? O6 Sn1 C25 107.2(2) . . ? O7 Sn1 C29 98.9(2) . . ? O6 Sn1 C29 105.7(2) . . ? C25 Sn1 C29 141.5(3) . . ? O7 Sn1 O6 169.05(13) . 2_566 ? O6 Sn1 O6 74.88(13) . 2_566 ? C25 Sn1 O6 84.82(19) . 2_566 ? C29 Sn1 O6 85.0(2) . 2_566 ? C32 C31 C30 115.1(15) . . ? C32 C31 H31A 108.5 . . ? C30 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? C30 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 C29 C30 1.427(11) . ? C29 Sn1 2.121(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C1 C6 1.354(9) . ? C1 C2 1.393(10) . ? C1 H1 0.9300 . ? C2 C3 1.332(13) . ? C2 H2 0.9300 . ? C3 C4 1.326(14) . ? C3 H3 0.9300 . ? C4 C5 1.389(10) . ? C4 H4 0.9300 . ? C5 C6 1.394(8) . ? C5 H5 0.9300 . ? C6 Si1 1.838(5) . ? C7 C12 1.385(8) . ? C7 C8 1.389(9) . ? C7 H7 0.9300 . ? C8 C9 1.348(10) . ? C8 H8 0.9300 . ? C9 C10 1.367(10) . ? C9 H9 0.9300 . ? C10 C11 1.388(8) . ? C10 H10 0.9300 . ? C11 C12 1.384(7) . ? C11 H11 0.9300 . ? C12 Si4 1.859(5) . ? C13 C18 1.355(9) . ? C13 C14 1.364(8) . ? C13 Si2 1.846(5) . ? C14 C15 1.404(10) . ? C14 H14 0.9300 . ? C15 C16 1.304(13) . ? C15 H15 0.9300 . ? C30 C31 1.540(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C16 C17 1.305(14) . ? C16 H16 0.9300 . ? C17 C18 1.410(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.351(10) . ? C19 C20 1.384(10) . ? C19 Si3 1.854(5) . ? C20 C21 1.393(11) . ? C20 H20 0.9300 . ? C21 C22 1.393(15) . ? C21 H21 0.9300 . ? C22 C23 1.310(14) . ? C22 H22 0.9300 . ? C23 C24 1.366(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.487(9) . ? C25 Sn1 2.112(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.529(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.510(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? O1 Si2 1.604(3) . ? O1 Si3 1.625(3) . ? O2 Si2 1.603(4) . ? O2 Si4 1.613(3) 2_666 ? O3 Si1 1.603(3) . ? O3 Si2 1.607(4) . ? O4 Si1 1.593(4) . ? O4 Si3 1.619(4) 2_666 ? O5 Si1 1.610(3) . ? O5 Si4 1.619(3) . ? O6 Si4 1.604(3) . ? O6 Sn1 2.026(3) . ? O6 Sn1 2.549(3) 2_566 ? O7 Si3 1.560(4) . ? O7 Sn1 1.995(4) . ? Si3 O4 1.619(4) 2_666 ? Si4 O2 1.613(3) 2_666 ? Sn1 O6 2.549(3) 2_566 ? C31 C32 1.397(16) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ?