#------------------------------------------------------------------------------ #$Date: 2019-06-05 03:19:39 +0300 (Wed, 05 Jun 2019) $ #$Revision: 215692 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551205.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_1551205 _journal_paper_doi 10.1039/C9SC01960J _chemical_formula_sum 'C56 H148 K N7 O8 Si12 Th2' _chemical_formula_weight 1888.07 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-04-18 deposited with the CCDC. 2019-06-04 downloaded from the CCDC. ; _cell_angle_alpha 74.546(15) _cell_angle_beta 71.051(15) _cell_angle_gamma 71.238(14) _cell_formula_units_Z 1 _cell_length_a 11.893(3) _cell_length_b 14.617(4) _cell_length_c 14.620(4) _cell_measurement_reflns_used 1777 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 18.6 _cell_measurement_theta_min 2.3 _cell_volume 2238.5(11) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_unetI/netI 0.1496 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 22425 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.700 _diffrn_reflns_theta_min 1.496 _exptl_absorpt_coefficient_mu 3.569 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6592 _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.400 _exptl_crystal_description block _exptl_crystal_F_000 964 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.246 _refine_diff_density_min -2.456 _refine_diff_density_rms 0.264 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 422 _refine_ls_number_reflns 9312 _refine_ls_number_restraints 1344 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0804 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+56.9818P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1803 _refine_ls_wR_factor_ref 0.1950 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6812 _reflns_number_total 9312 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc01960j2.cif _cod_data_source_block complex_K1 _cod_original_cell_volume 2238.6(10) _cod_database_code 1551205 _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 0.617 _shelx_estimated_absorpt_t_max multi-scan _shelx_res_file ; SLS499_0m_a.res created by SHELXL-2014/7 TITL SLS499_0m_a.res in P-1 CELL 0.71073 11.8932 14.6173 14.6203 74.546 71.051 71.238 ZERR 1.000 0.0030 0.0035 0.0035 0.015 0.015 0.014 LATT 1 SFAC C N O Si K Th H UNIT 56 7 8 12 1 2 148 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 sadi 0.01 C1 C2 C31 C32 C31 C33 C32 C33 C34 C35 C34 C36 C35 C36 sadi 0.01 C1 C2 C25 C26 C25 C27 C26 C27 C28 C29 C28 C30 C29 C30 sadi 0.01 C1 C2 C19 C20 C19 C21 C20 C21 C22 C23 C22 C24 C23 C24 sadi 0.01 C1 C2 C13 C14 C13 C15 C14 C15 C16 C17 C16 C18 C17 C18 sadi 0.01 C1 C2 C7 C8 C7 C9 C8 C9 C10 C11 C10 C12 C11 C12 sadi 0.01 C1 C2 C1 C3 C2 C3 C4 C5 C4 C6 C5 C6 sadi 0.01 Si1 C1 Si11 C31 Si11 C32 Si11 C33 Si12 C34 Si12 C35 Si12 C36 sadi 0.01 Si1 C1 Si9 C25 Si9 C26 Si9 C27 Si10 C28 Si10 C29 Si10 C30 sadi 0.01 Si1 C1 Si7 C19 Si7 C20 Si7 C21 Si8 C22 Si8 C23 Si8 C24 sadi 0.01 Si1 C1 Si5 C13 Si5 C14 Si5 C15 Si6 C16 Si6 C17 Si6 C18 sadi 0.01 Si1 C1 Si3 C7 Si3 C8 Si3 C9 Si4 C10 Si4 C11 Si4 C12 sadi 0.01 Si1 C1 Si1 C2 Si1 C3 Si2 C4 Si2 C5 Si2 C6 sadi 0.01 N2 Si1 N2 Si2 N2 Si3 N2 Si4 sadi 0.01 N2 Si1 N3 Si5 N3 Si6 N3 Si7 N3 Si8 sadi 0.01 N2 Si1 N4 Si9 N4 Si10 N4 Si11 N4 Si12 sadi 0.01 O1 C56 O1 C59 O1 C62 sadi 0.01 C56 C60 C56 C57 C57 C58 C60 C61 C58 C59 C61 C62 eadp C1 C35 C36 eadp C1 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32 C33 C34 eadp C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C18 C19 eadp C57 C60 eadp C58 C61 eadp C59 C62 size 0.15 0.15 0.1 TEMP -163.260 WGHT 0.000000 56.981804 FVAR 0.40666 PART 1 MOLE 1 SI1 4 0.317885 0.259418 0.997181 10.50000 0.01119 0.01588 = 0.02876 -0.00554 -0.01319 -0.00009 SI2 4 0.184795 0.133016 0.969898 10.50000 0.01349 0.00992 = 0.02522 0.00505 -0.01231 -0.00386 C1 1 0.328955 0.194021 1.123793 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H1A 7 0.259586 0.226815 1.172315 10.50000 -1.50000 H1B 7 0.406354 0.195181 1.133227 10.50000 -1.50000 H1C 7 0.326730 0.125772 1.132238 10.50000 -1.50000 AFIX 0 C2 1 0.474796 0.217372 0.914708 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H2A 7 0.480716 0.156832 0.894547 10.50000 -1.50000 H2B 7 0.537056 0.204872 0.950078 10.50000 -1.50000 H2C 7 0.488695 0.268419 0.856357 10.50000 -1.50000 AFIX 0 C3 1 0.298195 0.391839 0.995643 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H3A 7 0.308112 0.427956 0.927846 10.50000 -1.50000 H3B 7 0.360292 0.397878 1.022722 10.50000 -1.50000 H3C 7 0.215853 0.419142 1.035556 10.50000 -1.50000 AFIX 0 C4 1 0.115415 0.129998 0.873468 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H4A 7 0.037487 0.180833 0.876847 10.50000 -1.50000 H4B 7 0.100245 0.065380 0.884464 10.50000 -1.50000 H4C 7 0.172079 0.142194 0.808454 10.50000 -1.50000 AFIX 0 C5 1 0.332597 0.035056 0.955464 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H5A 7 0.388745 0.052182 0.891498 10.50000 -1.50000 H5B 7 0.316477 -0.027716 0.959325 10.50000 -1.50000 H5C 7 0.370148 0.029285 1.007995 10.50000 -1.50000 AFIX 0 C6 1 0.082362 0.090213 1.090188 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H6A 7 0.115131 0.089851 1.143771 10.50000 -1.50000 H6B 7 0.078603 0.023652 1.092333 10.50000 -1.50000 H6C 7 -0.000454 0.134653 1.097642 10.50000 -1.50000 AFIX 0 SI11 4 0.328837 0.413321 0.681356 10.50000 0.01907 0.03309 = 0.00943 0.00301 -0.00511 -0.00529 SI12 4 0.124158 0.592638 0.692131 10.50000 0.02428 0.01538 = 0.00917 0.00125 -0.00154 -0.00346 C31 1 0.359792 0.444488 0.544301 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H31A 7 0.401425 0.384387 0.516609 10.50000 -1.50000 H31B 7 0.412360 0.490180 0.518326 10.50000 -1.50000 H31C 7 0.281806 0.475222 0.526179 10.50000 -1.50000 AFIX 0 C32 1 0.457143 0.437753 0.710305 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H32A 7 0.440124 0.508234 0.708960 10.50000 -1.50000 H32B 7 0.534377 0.416564 0.661329 10.50000 -1.50000 H32C 7 0.464275 0.401284 0.775820 10.50000 -1.50000 AFIX 0 C33 1 0.350230 0.277715 0.713431 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H33A 7 0.325422 0.257830 0.785055 10.50000 -1.50000 H33B 7 0.436996 0.244753 0.688274 10.50000 -1.50000 H33C 7 0.299526 0.259237 0.683833 10.50000 -1.50000 AFIX 0 C34 1 0.222546 0.679707 0.660439 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H34A 7 0.226919 0.693606 0.720995 10.50000 -1.50000 H34B 7 0.186781 0.741024 0.620641 10.50000 -1.50000 H34C 7 0.305511 0.650129 0.623068 10.50000 -1.50000 AFIX 0 C35 1 -0.022665 0.647676 0.778569 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H35A 7 -0.090811 0.629339 0.770569 10.50000 -1.50000 H35B 7 -0.038035 0.719379 0.764053 10.50000 -1.50000 H35C 7 -0.016078 0.623146 0.846375 10.50000 -1.50000 AFIX 0 C36 1 0.082031 0.602811 0.576299 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H36A 7 0.155696 0.600233 0.520823 10.50000 -1.50000 H36B 7 0.020956 0.665262 0.564752 10.50000 -1.50000 H36C 7 0.047403 0.548260 0.582732 10.50000 -1.50000 AFIX 0 SI7 4 -0.203336 0.323629 0.967126 10.50000 0.01388 0.01546 = 0.01643 -0.00629 -0.00255 -0.00431 SI8 4 -0.114595 0.374554 0.752392 10.50000 0.02052 0.01365 = 0.01726 -0.00288 -0.01140 -0.00392 C19 1 -0.365857 0.395037 0.971252 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H19A 7 -0.376770 0.462602 0.977709 10.50000 -1.50000 H19B 7 -0.421579 0.364344 1.027705 10.50000 -1.50000 H19C 7 -0.384487 0.395630 0.910505 10.50000 -1.50000 AFIX 0 C20 1 -0.174542 0.334548 1.081469 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H20A 7 -0.100001 0.284628 1.092766 10.50000 -1.50000 H20B 7 -0.244819 0.324706 1.137512 10.50000 -1.50000 H20C 7 -0.163694 0.400040 1.074142 10.50000 -1.50000 AFIX 0 C21 1 -0.200969 0.192172 0.981987 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H21A 7 -0.220330 0.182796 0.925412 10.50000 -1.50000 H21B 7 -0.262267 0.174336 1.042369 10.50000 -1.50000 H21C 7 -0.119070 0.150395 0.985982 10.50000 -1.50000 AFIX 0 C22 1 -0.187315 0.282520 0.742769 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H22A 7 -0.144813 0.216459 0.770236 10.50000 -1.50000 H22B 7 -0.181006 0.285698 0.673530 10.50000 -1.50000 H22C 7 -0.274185 0.297232 0.779506 10.50000 -1.50000 AFIX 0 C23 1 0.035510 0.359137 0.656682 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H23A 7 0.066821 0.416892 0.644138 10.50000 -1.50000 H23B 7 0.023778 0.352110 0.595819 10.50000 -1.50000 H23C 7 0.094755 0.300312 0.679828 10.50000 -1.50000 AFIX 0 C24 1 -0.212200 0.497263 0.709626 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H24A 7 -0.290968 0.511108 0.759292 10.50000 -1.50000 H24B 7 -0.227011 0.497038 0.647554 10.50000 -1.50000 H24C 7 -0.169822 0.548013 0.699597 10.50000 -1.50000 PART 2 AFIX 0 SI3 4 0.328789 0.181505 0.912002 10.50000 0.03156 0.03568 = 0.06469 -0.00131 -0.01408 -0.00118 SI4 4 0.126476 0.191823 1.091037 10.50000 0.04046 0.02787 = 0.05062 -0.00208 -0.01624 -0.00352 C7 1 0.349819 0.213722 0.776254 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H7A 7 0.295106 0.187469 0.758564 10.50000 -1.50000 H7B 7 0.435441 0.185299 0.742941 10.50000 -1.50000 H7C 7 0.329958 0.285327 0.755930 10.50000 -1.50000 AFIX 0 C8 1 0.459296 0.208248 0.935229 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H8A 7 0.467940 0.273409 0.898539 10.50000 -1.50000 H8B 7 0.535470 0.158594 0.913667 10.50000 -1.50000 H8C 7 0.443032 0.206790 1.005681 10.50000 -1.50000 AFIX 0 C9 1 0.355269 0.045077 0.943644 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H9A 7 0.441270 0.014544 0.944977 10.50000 -1.50000 H9B 7 0.337276 0.022009 0.894139 10.50000 -1.50000 H9C 7 0.301155 0.027100 1.008416 10.50000 -1.50000 AFIX 0 C10 1 0.226210 0.163498 1.176381 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H10A 7 0.189279 0.126984 1.239818 10.50000 -1.50000 H10B 7 0.233498 0.224951 1.186073 10.50000 -1.50000 H10C 7 0.308057 0.123731 1.147925 10.50000 -1.50000 AFIX 0 C11 1 -0.021090 0.276528 1.146855 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H11A 7 -0.013576 0.344293 1.126089 10.50000 -1.50000 H11B 7 -0.039209 0.258864 1.218690 10.50000 -1.50000 H11C 7 -0.087900 0.270863 1.125070 10.50000 -1.50000 AFIX 0 C12 1 0.088124 0.074282 1.102124 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H12A 7 0.110770 0.057613 1.036740 10.50000 -1.50000 H12B 7 -0.000373 0.082011 1.131387 10.50000 -1.50000 H12C 7 0.133868 0.021597 1.144057 10.50000 -1.50000 AFIX 0 SI5 4 -0.116241 0.252788 0.875041 10.50000 0.02494 0.03477 = 0.05515 -0.01062 -0.01095 -0.00952 SI6 4 -0.203429 0.466924 0.823337 10.50000 0.02984 0.03892 = 0.04127 -0.01049 -0.01222 -0.00720 C13 1 0.035545 0.159091 0.858523 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H13A 7 0.087141 0.174986 0.791988 10.50000 -1.50000 H13B 7 0.022525 0.093928 0.868141 10.50000 -1.50000 H13C 7 0.076530 0.159249 0.906784 10.50000 -1.50000 AFIX 0 C14 1 -0.185943 0.243764 0.780970 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H14A 7 -0.272329 0.243202 0.811469 10.50000 -1.50000 H14B 7 -0.140967 0.183033 0.755016 10.50000 -1.50000 H14C 7 -0.181027 0.300333 0.727174 10.50000 -1.50000 AFIX 0 C15 1 -0.213423 0.205556 0.996559 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H15A 7 -0.173987 0.198139 1.048393 10.50000 -1.50000 H15B 7 -0.222513 0.141691 0.995127 10.50000 -1.50000 H15C 7 -0.294714 0.252077 1.009858 10.50000 -1.50000 AFIX 0 C16 1 -0.173552 0.580635 0.834706 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H16A 7 -0.152695 0.569963 0.896961 10.50000 -1.50000 H16B 7 -0.247363 0.635239 0.833285 10.50000 -1.50000 H16C 7 -0.104908 0.596420 0.779842 10.50000 -1.50000 AFIX 0 C17 1 -0.365626 0.470321 0.896626 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H17A 7 -0.365997 0.415918 0.952893 10.50000 -1.50000 H17B 7 -0.411963 0.463991 0.855121 10.50000 -1.50000 H17C 7 -0.403930 0.532835 0.920277 10.50000 -1.50000 AFIX 0 C18 1 -0.203693 0.483501 0.692219 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H18A 7 -0.129430 0.502721 0.649055 10.50000 -1.50000 H18B 7 -0.276660 0.534856 0.679775 10.50000 -1.50000 H18C 7 -0.205126 0.421625 0.679040 10.50000 -1.50000 AFIX 0 SI9 4 0.185134 0.469591 0.632313 10.50000 0.02633 0.04622 = 0.03595 -0.00450 -0.00849 -0.01289 SI10 4 0.318072 0.496885 0.759109 10.50000 0.02382 0.04615 = 0.04099 -0.00783 -0.00631 -0.01391 C25 1 0.114651 0.373361 0.629842 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H25A 7 0.168673 0.308171 0.645820 10.50000 -1.50000 H25B 7 0.103887 0.382008 0.564120 10.50000 -1.50000 H25C 7 0.034407 0.379408 0.678289 10.50000 -1.50000 AFIX 0 C26 1 0.335663 0.452033 0.537083 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H26A 7 0.369550 0.508191 0.525696 10.50000 -1.50000 H26B 7 0.323363 0.447050 0.475652 10.50000 -1.50000 H26C 7 0.393093 0.391639 0.559913 10.50000 -1.50000 AFIX 0 C27 1 0.086526 0.589575 0.585624 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H27A 7 0.006105 0.602857 0.633482 10.50000 -1.50000 H27B 7 0.075537 0.586920 0.522873 10.50000 -1.50000 H27C 7 0.126105 0.642015 0.575977 10.50000 -1.50000 AFIX 0 C28 1 0.329695 0.623703 0.693906 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H28A 7 0.322907 0.633627 0.626723 10.50000 -1.50000 H28B 7 0.409192 0.631876 0.691742 10.50000 -1.50000 H28C 7 0.263074 0.672021 0.729108 10.50000 -1.50000 AFIX 0 C29 1 0.474617 0.414912 0.715369 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H29A 7 0.491600 0.359048 0.768040 10.50000 -1.50000 H29B 7 0.536594 0.451967 0.697245 10.50000 -1.50000 H29C 7 0.477531 0.390848 0.657945 10.50000 -1.50000 AFIX 0 C30 1 0.300644 0.494959 0.891434 10.50000 0.03468 0.03700 = 0.04087 -0.00381 -0.01048 -0.01021 AFIX 137 H30A 7 0.217000 0.531339 0.920755 10.50000 -1.50000 H30B 7 0.360097 0.525700 0.896249 10.50000 -1.50000 H30C 7 0.315708 0.426831 0.926606 10.50000 -1.50000 PART 3 AFIX 0 C59 1 0.366562 0.964045 0.319472 10.50000 0.07138 AFIX 23 H59A 7 0.436282 0.935050 0.267547 10.50000 -1.20000 H59B 7 0.357716 1.035678 0.306763 10.50000 -1.20000 AFIX 0 C58 1 0.249520 0.944237 0.319484 10.50000 0.06289 AFIX 23 H58A 7 0.262419 0.910239 0.265292 10.50000 -1.20000 H58B 7 0.182372 1.005235 0.315737 10.50000 -1.20000 AFIX 0 C57 1 0.225379 0.878192 0.418717 10.50000 0.09501 AFIX 23 H57A 7 0.196854 0.823669 0.413425 10.50000 -1.20000 H57B 7 0.159051 0.916088 0.466250 10.50000 -1.20000 PART 4 AFIX 0 C61 1 0.205517 0.913549 0.395343 10.50000 0.06289 AFIX 23 H61A 7 0.148197 0.955577 0.443121 10.50000 -1.20000 H61B 7 0.162784 0.918515 0.345623 10.50000 -1.20000 AFIX 0 C62 1 0.316239 0.954542 0.344306 10.50000 0.07138 AFIX 23 H62A 7 0.362478 0.929328 0.282461 10.50000 -1.20000 H62B 7 0.291472 1.027225 0.329302 10.50000 -1.20000 AFIX 0 C60 1 0.231256 0.808599 0.448955 10.50000 0.09501 AFIX 23 H60A 7 0.170162 0.794979 0.512141 10.50000 -1.20000 H60B 7 0.252776 0.758336 0.407888 10.50000 -1.20000 PART 0 AFIX 0 C55 1 0.558458 0.766892 0.667670 11.00000 0.03130 0.05400 = 0.10981 0.04469 0.00173 0.00654 AFIX 23 H55A 7 0.606586 0.717777 0.711378 11.00000 -1.20000 H55B 7 0.537001 0.731580 0.629221 11.00000 -1.20000 AFIX 0 C54 1 0.738722 0.782793 0.543334 11.00000 0.03191 0.03906 = 0.05472 0.00120 -0.00725 -0.00513 AFIX 23 H54A 7 0.719179 0.748686 0.502592 11.00000 -1.20000 H54B 7 0.788678 0.732597 0.585068 11.00000 -1.20000 AFIX 0 C53 1 0.809181 0.850210 0.480135 11.00000 0.01441 0.03202 = 0.03990 0.00065 -0.00509 0.00130 AFIX 23 H53A 7 0.823073 0.888471 0.520201 11.00000 -1.20000 H53B 7 0.890384 0.813053 0.445053 11.00000 -1.20000 AFIX 0 C52 1 0.812162 0.981608 0.349743 11.00000 0.03022 0.03525 = 0.02936 -0.00761 -0.00668 -0.00580 AFIX 23 H52A 7 0.892634 0.946899 0.311251 11.00000 -1.20000 H52B 7 0.827125 1.020470 0.388615 11.00000 -1.20000 AFIX 0 C51 1 0.736358 1.047610 0.282442 11.00000 0.03396 0.05436 = 0.02757 -0.00933 0.00082 -0.00111 AFIX 23 H51A 7 0.785405 1.089319 0.230745 11.00000 -1.20000 H51B 7 0.713414 1.007475 0.249944 11.00000 -1.20000 AFIX 0 C50 1 0.557433 1.173627 0.271738 11.00000 0.06621 0.07048 = 0.06531 0.05261 0.00390 0.00489 AFIX 23 H50A 7 0.535463 1.136638 0.235260 11.00000 -1.20000 H50B 7 0.605180 1.218228 0.223285 11.00000 -1.20000 AFIX 0 C56 1 0.339100 0.836253 0.456642 11.00000 0.09796 AFIX 23 H56A 7 0.319214 0.822397 0.529363 11.00000 -1.20000 H56B 7 0.393719 0.776759 0.430225 11.00000 -1.20000 AFIX 0 K002 5 0.500000 1.000000 0.500000 10.50000 0.03109 0.03099 = 0.03773 0.00187 -0.00655 -0.00307 N1 2 0.000000 0.500000 1.000000 10.50000 0.02233 0.02385 = 0.02050 0.00576 -0.01895 -0.01031 N2 2 0.189747 0.248435 0.972555 11.00000 0.02304 0.01037 = 0.04615 0.00055 -0.02196 -0.00003 N3 2 -0.095991 0.366592 0.866252 11.00000 0.01679 0.02636 = 0.03405 -0.01553 -0.01064 -0.00625 N4 2 0.188943 0.473768 0.747571 11.00000 0.02159 0.04332 = 0.02170 -0.00400 -0.00979 -0.01136 O3 3 0.747592 0.913587 0.412533 11.00000 0.02229 0.03070 = 0.03451 -0.00005 -0.00841 -0.00467 O1 3 0.388293 0.920168 0.414518 11.00000 0.11279 0.06291 = 0.06653 -0.00469 -0.03430 -0.04198 O2 3 0.630011 1.107217 0.333762 11.00000 0.03467 0.05044 = 0.02477 0.01289 -0.00128 -0.00067 O4 3 0.628407 0.831142 0.603912 11.00000 0.03033 0.03144 = 0.05611 0.00922 0.00213 -0.00280 TH01 6 0.069074 0.400947 0.900246 11.00000 0.01522 0.01632 = 0.01928 -0.00200 -0.00638 -0.00381 HKLF 4 REM SLS499_0m_a.res in P-1 REM R1 = 0.0804 for 6812 Fo > 4sig(Fo) and 0.1177 for all 9312 data REM 422 parameters refined using 1344 restraints END WGHT 0.0000 57.6213 REM Highest difference peak 1.246, deepest hole -2.456, 1-sigma level 0.264 Q1 1 0.1968 0.4478 0.7445 11.00000 0.05 1.25 Q2 1 0.3318 0.2764 0.7025 11.00000 0.05 1.24 Q3 1 0.2033 0.2373 0.9477 11.00000 0.05 1.07 Q4 1 0.7126 0.8754 0.3727 11.00000 0.05 1.05 Q5 1 0.0812 0.3809 0.8755 11.00000 0.05 1.04 Q6 1 -0.0819 0.3437 0.5783 11.00000 0.05 1.02 Q7 1 0.6194 0.1585 1.0150 11.00000 0.05 0.97 Q8 1 0.5441 0.9057 0.2303 11.00000 0.05 0.94 Q9 1 -0.0015 0.3994 0.8479 11.00000 0.05 0.94 Q10 1 -0.0818 0.1611 1.1325 11.00000 0.05 0.93 Q11 1 0.8205 1.1820 0.1780 11.00000 0.05 0.93 Q12 1 0.6089 0.5075 0.6217 11.00000 0.05 0.92 Q13 1 0.4385 0.2462 0.6472 11.00000 0.05 0.92 Q14 1 0.8374 0.8836 0.5932 11.00000 0.05 0.92 Q15 1 0.2516 0.6595 0.6524 11.00000 0.05 0.91 Q16 1 0.3023 0.9984 0.2856 11.00000 0.05 0.91 Q17 1 0.0008 0.3621 0.9967 11.00000 0.05 0.90 Q18 1 0.1845 0.9650 0.3498 11.00000 0.05 0.90 Q19 1 0.3127 0.3997 0.9650 11.00000 0.05 0.90 Q20 1 0.4785 1.0803 0.2408 11.00000 0.05 0.89 ; _shelx_res_checksum 20422 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 Si1 Si 0.3179(6) 0.2594(5) 0.9972(5) 0.0171(15) Uani 0.5 1 d D . P A 1 Si2 Si 0.1848(6) 0.1330(4) 0.9699(5) 0.0158(15) Uani 0.5 1 d D . P A 1 C1 C 0.329(2) 0.1940(16) 1.1238(10) 0.0378(12) Uani 0.5 1 d D . P A 1 H1A H 0.2596 0.2268 1.1723 0.057 Uiso 0.5 1 calc R U P A 1 H1B H 0.4064 0.1952 1.1332 0.057 Uiso 0.5 1 calc R U P A 1 H1C H 0.3267 0.1258 1.1322 0.057 Uiso 0.5 1 calc R U P A 1 C2 C 0.4748(14) 0.2174(17) 0.9147(16) 0.0378(12) Uani 0.5 1 d D . P A 1 H2A H 0.4807 0.1568 0.8945 0.057 Uiso 0.5 1 calc R U P A 1 H2B H 0.5371 0.2049 0.9501 0.057 Uiso 0.5 1 calc R U P A 1 H2C H 0.4887 0.2684 0.8564 0.057 Uiso 0.5 1 calc R U P A 1 C3 C 0.298(2) 0.3918(8) 0.9956(17) 0.0378(12) Uani 0.5 1 d D . P A 1 H3A H 0.3081 0.4280 0.9278 0.057 Uiso 0.5 1 calc R U P A 1 H3B H 0.3603 0.3979 1.0227 0.057 Uiso 0.5 1 calc R U P A 1 H3C H 0.2159 0.4191 1.0356 0.057 Uiso 0.5 1 calc R U P A 1 C4 C 0.115(2) 0.130(2) 0.8735(14) 0.0378(12) Uani 0.5 1 d D . P A 1 H4A H 0.0375 0.1808 0.8768 0.057 Uiso 0.5 1 calc R U P A 1 H4B H 0.1002 0.0654 0.8845 0.057 Uiso 0.5 1 calc R U P A 1 H4C H 0.1721 0.1422 0.8085 0.057 Uiso 0.5 1 calc R U P A 1 C5 C 0.3326(14) 0.0351(16) 0.9555(18) 0.0378(12) Uani 0.5 1 d D . P A 1 H5A H 0.3887 0.0522 0.8915 0.057 Uiso 0.5 1 calc R U P A 1 H5B H 0.3165 -0.0277 0.9593 0.057 Uiso 0.5 1 calc R U P A 1 H5C H 0.3701 0.0293 1.0080 0.057 Uiso 0.5 1 calc R U P A 1 C6 C 0.0824(19) 0.090(2) 1.0902(11) 0.0378(12) Uani 0.5 1 d D . P A 1 H6A H 0.1151 0.0899 1.1438 0.057 Uiso 0.5 1 calc R U P A 1 H6B H 0.0786 0.0237 1.0923 0.057 Uiso 0.5 1 calc R U P A 1 H6C H -0.0005 0.1347 1.0976 0.057 Uiso 0.5 1 calc R U P A 1 Si11 Si 0.3288(6) 0.4133(5) 0.6814(5) 0.0219(16) Uani 0.5 1 d D . P B 1 Si12 Si 0.1242(6) 0.5926(5) 0.6921(5) 0.0181(15) Uani 0.5 1 d D . P B 1 C31 C 0.360(3) 0.444(2) 0.5443(8) 0.0378(12) Uani 0.5 1 d D . P B 1 H31A H 0.4014 0.3844 0.5166 0.057 Uiso 0.5 1 calc R U P B 1 H31B H 0.4124 0.4902 0.5183 0.057 Uiso 0.5 1 calc R U P B 1 H31C H 0.2818 0.4752 0.5262 0.057 Uiso 0.5 1 calc R U P B 1 C32 C 0.457(2) 0.4378(18) 0.7103(19) 0.0378(12) Uani 0.5 1 d D . P B 1 H32A H 0.4401 0.5082 0.7090 0.057 Uiso 0.5 1 calc R U P B 1 H32B H 0.5344 0.4166 0.6613 0.057 Uiso 0.5 1 calc R U P B 1 H32C H 0.4643 0.4013 0.7758 0.057 Uiso 0.5 1 calc R U P B 1 C33 C 0.350(3) 0.2777(9) 0.7134(19) 0.0378(12) Uani 0.5 1 d D . P B 1 H33A H 0.3254 0.2578 0.7851 0.057 Uiso 0.5 1 calc R U P B 1 H33B H 0.4370 0.2448 0.6883 0.057 Uiso 0.5 1 calc R U P B 1 H33C H 0.2995 0.2592 0.6838 0.057 Uiso 0.5 1 calc R U P B 1 C34 C 0.2225(19) 0.6797(16) 0.6604(18) 0.0378(12) Uani 0.5 1 d D . P B 1 H34A H 0.2269 0.6936 0.7210 0.057 Uiso 0.5 1 calc R U P B 1 H34B H 0.1868 0.7410 0.6206 0.057 Uiso 0.5 1 calc R U P B 1 H34C H 0.3055 0.6501 0.6231 0.057 Uiso 0.5 1 calc R U P B 1 C35 C -0.0227(14) 0.6477(18) 0.7786(15) 0.0378(12) Uani 0.5 1 d D . P B 1 H35A H -0.0908 0.6293 0.7706 0.057 Uiso 0.5 1 calc R U P B 1 H35B H -0.0380 0.7194 0.7641 0.057 Uiso 0.5 1 calc R U P B 1 H35C H -0.0161 0.6231 0.8464 0.057 Uiso 0.5 1 calc R U P B 1 C36 C 0.082(2) 0.603(2) 0.5763(12) 0.0378(12) Uani 0.5 1 d D . P B 1 H36A H 0.1557 0.6002 0.5208 0.057 Uiso 0.5 1 calc R U P B 1 H36B H 0.0210 0.6653 0.5648 0.057 Uiso 0.5 1 calc R U P B 1 H36C H 0.0474 0.5483 0.5827 0.057 Uiso 0.5 1 calc R U P B 1 Si7 Si -0.2033(6) 0.3236(5) 0.9671(4) 0.0148(14) Uani 0.5 1 d D . P C 1 Si8 Si -0.1146(6) 0.3746(5) 0.7524(4) 0.0156(15) Uani 0.5 1 d D . P C 1 C19 C -0.3659(13) 0.3950(16) 0.971(2) 0.0378(12) Uani 0.5 1 d D . P C 1 H19A H -0.3768 0.4626 0.9777 0.057 Uiso 0.5 1 calc R U P C 1 H19B H -0.4216 0.3643 1.0277 0.057 Uiso 0.5 1 calc R U P C 1 H19C H -0.3845 0.3956 0.9105 0.057 Uiso 0.5 1 calc R U P C 1 C20 C -0.175(2) 0.3345(17) 1.0815(14) 0.0378(12) Uani 0.5 1 d D . P C 1 H20A H -0.1000 0.2846 1.0928 0.057 Uiso 0.5 1 calc R U P C 1 H20B H -0.2448 0.3247 1.1375 0.057 Uiso 0.5 1 calc R U P C 1 H20C H -0.1637 0.4000 1.0741 0.057 Uiso 0.5 1 calc R U P C 1 C21 C -0.201(3) 0.1922(9) 0.982(2) 0.0378(12) Uani 0.5 1 d D . P C 1 H21A H -0.2203 0.1828 0.9254 0.057 Uiso 0.5 1 calc R U P C 1 H21B H -0.2623 0.1743 1.0424 0.057 Uiso 0.5 1 calc R U P C 1 H21C H -0.1191 0.1504 0.9860 0.057 Uiso 0.5 1 calc R U P C 1 C22 C -0.187(2) 0.2825(14) 0.743(2) 0.0378(12) Uani 0.5 1 d D . P C 1 H22A H -0.1448 0.2165 0.7702 0.057 Uiso 0.5 1 calc R U P C 1 H22B H -0.1810 0.2857 0.6735 0.057 Uiso 0.5 1 calc R U P C 1 H22C H -0.2742 0.2972 0.7795 0.057 Uiso 0.5 1 calc R U P C 1 C23 C 0.0355(14) 0.3591(17) 0.6567(17) 0.0378(12) Uani 0.5 1 d D . P C 1 H23A H 0.0668 0.4169 0.6441 0.057 Uiso 0.5 1 calc R U P C 1 H23B H 0.0238 0.3521 0.5958 0.057 Uiso 0.5 1 calc R U P C 1 H23C H 0.0948 0.3003 0.6798 0.057 Uiso 0.5 1 calc R U P C 1 C24 C -0.212(2) 0.4973(10) 0.710(2) 0.0378(12) Uani 0.5 1 d D . P C 1 H24A H -0.2910 0.5111 0.7593 0.057 Uiso 0.5 1 calc R U P C 1 H24B H -0.2270 0.4970 0.6476 0.057 Uiso 0.5 1 calc R U P C 1 H24C H -0.1698 0.5480 0.6996 0.057 Uiso 0.5 1 calc R U P C 1 Si3 Si 0.3288(7) 0.1815(6) 0.9120(7) 0.047(3) Uani 0.5 1 d D . P A 2 Si4 Si 0.1265(8) 0.1918(6) 1.0910(6) 0.041(2) Uani 0.5 1 d D . P A 2 C7 C 0.350(3) 0.2137(18) 0.7763(10) 0.0378(12) Uani 0.5 1 d D . P A 2 H7A H 0.2951 0.1875 0.7586 0.057 Uiso 0.5 1 calc R U P A 2 H7B H 0.4354 0.1853 0.7429 0.057 Uiso 0.5 1 calc R U P A 2 H7C H 0.3300 0.2853 0.7559 0.057 Uiso 0.5 1 calc R U P A 2 C8 C 0.459(2) 0.2082(19) 0.9352(19) 0.0378(12) Uani 0.5 1 d D . P A 2 H8A H 0.4679 0.2734 0.8985 0.057 Uiso 0.5 1 calc R U P A 2 H8B H 0.5355 0.1586 0.9137 0.057 Uiso 0.5 1 calc R U P A 2 H8C H 0.4430 0.2068 1.0057 0.057 Uiso 0.5 1 calc R U P A 2 C9 C 0.355(3) 0.0451(9) 0.9436(19) 0.0378(12) Uani 0.5 1 d D . P A 2 H9A H 0.4413 0.0145 0.9450 0.057 Uiso 0.5 1 calc R U P A 2 H9B H 0.3373 0.0220 0.8941 0.057 Uiso 0.5 1 calc R U P A 2 H9C H 0.3012 0.0271 1.0084 0.057 Uiso 0.5 1 calc R U P A 2 C10 C 0.226(2) 0.1635(18) 1.1764(17) 0.0378(12) Uani 0.5 1 d D . P A 2 H10A H 0.1893 0.1270 1.2398 0.057 Uiso 0.5 1 calc R U P A 2 H10B H 0.2335 0.2250 1.1861 0.057 Uiso 0.5 1 calc R U P A 2 H10C H 0.3081 0.1237 1.1479 0.057 Uiso 0.5 1 calc R U P A 2 C11 C -0.0211(15) 0.2765(15) 1.1469(19) 0.0378(12) Uani 0.5 1 d D . P A 2 H11A H -0.0136 0.3443 1.1261 0.057 Uiso 0.5 1 calc R U P A 2 H11B H -0.0392 0.2589 1.2187 0.057 Uiso 0.5 1 calc R U P A 2 H11C H -0.0879 0.2709 1.1251 0.057 Uiso 0.5 1 calc R U P A 2 C12 C 0.088(2) 0.0743(12) 1.102(2) 0.0378(12) Uani 0.5 1 d D . P A 2 H12A H 0.1108 0.0576 1.0367 0.057 Uiso 0.5 1 calc R U P A 2 H12B H -0.0004 0.0820 1.1314 0.057 Uiso 0.5 1 calc R U P A 2 H12C H 0.1339 0.0216 1.1441 0.057 Uiso 0.5 1 calc R U P A 2 Si5 Si -0.1162(8) 0.2528(5) 0.8750(7) 0.037(2) Uani 0.5 1 d D . P C 2 Si6 Si -0.2034(7) 0.4669(6) 0.8233(6) 0.036(2) Uani 0.5 1 d D . P C 2 C13 C 0.0355(14) 0.1591(17) 0.8585(18) 0.0378(12) Uani 0.5 1 d D . P C 2 H13A H 0.0871 0.1750 0.7920 0.057 Uiso 0.5 1 calc R U P C 2 H13B H 0.0225 0.0939 0.8681 0.057 Uiso 0.5 1 calc R U P C 2 H13C H 0.0765 0.1592 0.9068 0.057 Uiso 0.5 1 calc R U P C 2 C14 C -0.186(2) 0.244(2) 0.7810(14) 0.0378(12) Uani 0.5 1 d D . P C 2 H14A H -0.2723 0.2432 0.8115 0.057 Uiso 0.5 1 calc R U P C 2 H14B H -0.1410 0.1830 0.7550 0.057 Uiso 0.5 1 calc R U P C 2 H14C H -0.1810 0.3003 0.7272 0.057 Uiso 0.5 1 calc R U P C 2 C15 C -0.213(2) 0.206(2) 0.9966(11) 0.0378(12) Uani 0.5 1 d D . P C 2 H15A H -0.1740 0.1981 1.0484 0.057 Uiso 0.5 1 calc R U P C 2 H15B H -0.2225 0.1417 0.9951 0.057 Uiso 0.5 1 calc R U P C 2 H15C H -0.2947 0.2521 1.0099 0.057 Uiso 0.5 1 calc R U P C 2 C16 C -0.174(2) 0.5806(14) 0.8347(18) 0.0378(12) Uani 0.5 1 d D . P C 2 H16A H -0.1527 0.5700 0.8970 0.057 Uiso 0.5 1 calc R U P C 2 H16B H -0.2474 0.6352 0.8333 0.057 Uiso 0.5 1 calc R U P C 2 H16C H -0.1049 0.5964 0.7798 0.057 Uiso 0.5 1 calc R U P C 2 C17 C -0.3656(14) 0.4703(19) 0.8966(16) 0.0378(12) Uani 0.5 1 d D . P C 2 H17A H -0.3660 0.4159 0.9529 0.057 Uiso 0.5 1 calc R U P C 2 H17B H -0.4120 0.4640 0.8551 0.057 Uiso 0.5 1 calc R U P C 2 H17C H -0.4039 0.5328 0.9203 0.057 Uiso 0.5 1 calc R U P C 2 C18 C -0.204(2) 0.484(2) 0.6922(9) 0.0378(12) Uani 0.5 1 d D . P C 2 H18A H -0.1294 0.5027 0.6491 0.057 Uiso 0.5 1 calc R U P C 2 H18B H -0.2767 0.5349 0.6798 0.057 Uiso 0.5 1 calc R U P C 2 H18C H -0.2051 0.4216 0.6790 0.057 Uiso 0.5 1 calc R U P C 2 Si9 Si 0.1851(8) 0.4696(7) 0.6323(5) 0.036(2) Uani 0.5 1 d D . P B 2 Si10 Si 0.3181(7) 0.4969(6) 0.7591(6) 0.036(2) Uani 0.5 1 d D . P A 2 C25 C 0.115(2) 0.3734(14) 0.630(2) 0.0378(12) Uani 0.5 1 d D . P B 2 H25A H 0.1687 0.3082 0.6458 0.057 Uiso 0.5 1 calc R U P B 2 H25B H 0.1039 0.3820 0.5641 0.057 Uiso 0.5 1 calc R U P B 2 H25C H 0.0344 0.3794 0.6783 0.057 Uiso 0.5 1 calc R U P B 2 C26 C 0.3357(14) 0.4520(19) 0.5371(17) 0.0378(12) Uani 0.5 1 d D . P B 2 H26A H 0.3695 0.5082 0.5257 0.057 Uiso 0.5 1 calc R U P B 2 H26B H 0.3234 0.4471 0.4757 0.057 Uiso 0.5 1 calc R U P B 2 H26C H 0.3931 0.3916 0.5599 0.057 Uiso 0.5 1 calc R U P B 2 C27 C 0.087(2) 0.5896(11) 0.586(2) 0.0378(12) Uani 0.5 1 d D . P B 2 H27A H 0.0061 0.6029 0.6335 0.057 Uiso 0.5 1 calc R U P B 2 H27B H 0.0755 0.5869 0.5229 0.057 Uiso 0.5 1 calc R U P B 2 H27C H 0.1261 0.6420 0.5760 0.057 Uiso 0.5 1 calc R U P B 2 C28 C 0.330(2) 0.6237(10) 0.6939(16) 0.0378(12) Uani 0.5 1 d D . P A 2 H28A H 0.3229 0.6336 0.6267 0.057 Uiso 0.5 1 calc R U P A 2 H28B H 0.4092 0.6319 0.6917 0.057 Uiso 0.5 1 calc R U P A 2 H28C H 0.2631 0.6720 0.7291 0.057 Uiso 0.5 1 calc R U P A 2 C29 C 0.4746(15) 0.4149(16) 0.7154(17) 0.0378(12) Uani 0.5 1 d D . P A 2 H29A H 0.4916 0.3590 0.7680 0.057 Uiso 0.5 1 calc R U P A 2 H29B H 0.5366 0.4520 0.6972 0.057 Uiso 0.5 1 calc R U P A 2 H29C H 0.4775 0.3908 0.6579 0.057 Uiso 0.5 1 calc R U P A 2 C30 C 0.301(2) 0.4950(17) 0.8914(9) 0.0378(12) Uani 0.5 1 d D . P A 2 H30A H 0.2170 0.5313 0.9208 0.057 Uiso 0.5 1 calc R U P A 2 H30B H 0.3601 0.5257 0.8962 0.057 Uiso 0.5 1 calc R U P A 2 H30C H 0.3157 0.4268 0.9266 0.057 Uiso 0.5 1 calc R U P A 2 C59 C 0.367(4) 0.964(3) 0.319(2) 0.071(9) Uiso 0.5 1 d D . P D 3 H59A H 0.4363 0.9351 0.2675 0.086 Uiso 0.5 1 calc R U P D 3 H59B H 0.3577 1.0357 0.3068 0.086 Uiso 0.5 1 calc R U P D 3 C58 C 0.250(3) 0.944(3) 0.319(3) 0.063(8) Uiso 0.5 1 d D . P D 3 H58A H 0.2624 0.9102 0.2653 0.075 Uiso 0.5 1 calc R U P D 3 H58B H 0.1824 1.0052 0.3157 0.075 Uiso 0.5 1 calc R U P D 3 C57 C 0.225(4) 0.878(5) 0.419(3) 0.095(13) Uiso 0.5 1 d D . P D 3 H57A H 0.1969 0.8237 0.4134 0.114 Uiso 0.5 1 calc R U P D 3 H57B H 0.1591 0.9161 0.4662 0.114 Uiso 0.5 1 calc R U P D 3 C61 C 0.206(3) 0.914(3) 0.395(4) 0.063(8) Uiso 0.5 1 d D . P D 4 H61A H 0.1482 0.9556 0.4431 0.075 Uiso 0.5 1 calc R U P D 4 H61B H 0.1628 0.9185 0.3456 0.075 Uiso 0.5 1 calc R U P D 4 C62 C 0.316(4) 0.955(4) 0.344(3) 0.071(9) Uiso 0.5 1 d D . P D 4 H62A H 0.3625 0.9293 0.2825 0.086 Uiso 0.5 1 calc R U P D 4 H62B H 0.2915 1.0272 0.3293 0.086 Uiso 0.5 1 calc R U P D 4 C60 C 0.231(3) 0.809(3) 0.449(4) 0.095(13) Uiso 0.5 1 d D . P D 4 H60A H 0.1702 0.7950 0.5121 0.114 Uiso 0.5 1 calc R U P D 4 H60B H 0.2528 0.7583 0.4079 0.114 Uiso 0.5 1 calc R U P D 4 C55 C 0.5585(17) 0.7669(15) 0.6677(18) 0.087(9) Uani 1 1 d . . . . . H55A H 0.6066 0.7178 0.7114 0.104 Uiso 1 1 calc R U . . . H55B H 0.5370 0.7316 0.6292 0.104 Uiso 1 1 calc R U . . . C54 C 0.7387(15) 0.7828(12) 0.5433(13) 0.046(4) Uani 1 1 d . . . . . H54A H 0.7192 0.7487 0.5026 0.055 Uiso 1 1 calc R U . . . H54B H 0.7887 0.7326 0.5851 0.055 Uiso 1 1 calc R U . . . C53 C 0.8092(13) 0.8502(11) 0.4801(11) 0.033(4) Uani 1 1 d . . . . . H53A H 0.8231 0.8885 0.5202 0.039 Uiso 1 1 calc R U . . . H53B H 0.8904 0.8131 0.4451 0.039 Uiso 1 1 calc R U . . . C52 C 0.8122(14) 0.9816(11) 0.3497(11) 0.032(4) Uani 1 1 d . . . . . H52A H 0.8926 0.9469 0.3113 0.039 Uiso 1 1 calc R U . . . H52B H 0.8271 1.0205 0.3886 0.039 Uiso 1 1 calc R U . . . C51 C 0.7364(15) 1.0476(13) 0.2824(11) 0.043(4) Uani 1 1 d . . . . . H51A H 0.7854 1.0893 0.2307 0.052 Uiso 1 1 calc R U . . . H51B H 0.7134 1.0075 0.2499 0.052 Uiso 1 1 calc R U . . . C50 C 0.557(2) 1.1736(16) 0.2717(16) 0.092(9) Uani 1 1 d . . . . . H50A H 0.5355 1.1366 0.2353 0.110 Uiso 1 1 calc R U . . . H50B H 0.6052 1.2182 0.2233 0.110 Uiso 1 1 calc R U . . . C56 C 0.339(2) 0.8363(17) 0.457(2) 0.098(9) Uiso 1 1 d D . . . . H56A H 0.3192 0.8224 0.5294 0.118 Uiso 1 1 calc R U . D 3 H56B H 0.3937 0.7768 0.4302 0.118 Uiso 1 1 calc R U . D 3 K002 K 0.5000 1.0000 0.5000 0.0368(12) Uani 1 2 d S . P D . N1 N 0.0000 0.5000 1.0000 0.020(3) Uani 1 2 d S . P A . N2 N 0.1897(7) 0.2484(6) 0.9726(6) 0.025(3) Uani 1 1 d D . . . . N3 N -0.0960(8) 0.3666(5) 0.8663(5) 0.022(3) Uani 1 1 d D . . . . N4 N 0.1889(7) 0.4738(6) 0.7476(6) 0.027(3) Uani 1 1 d D . . . . O3 O 0.7476(9) 0.9136(7) 0.4125(7) 0.031(2) Uani 1 1 d . . . . . O1 O 0.3883(15) 0.9202(10) 0.4145(10) 0.075(5) Uani 1 1 d D . . . . O2 O 0.6300(10) 1.1072(8) 0.3338(8) 0.045(3) Uani 1 1 d . . . . . O4 O 0.6284(10) 0.8311(8) 0.6039(9) 0.048(3) Uani 1 1 d . . . . . Th01 Th 0.06907(5) 0.40095(4) 0.90025(4) 0.01678(14) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.011(3) 0.016(4) 0.029(4) -0.006(3) -0.013(3) 0.000(3) Si2 0.013(3) 0.010(3) 0.025(4) 0.005(3) -0.012(3) -0.004(3) C1 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C2 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C3 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C4 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C5 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C6 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) Si11 0.019(4) 0.033(4) 0.009(3) 0.003(3) -0.005(3) -0.005(3) Si12 0.024(4) 0.015(4) 0.009(3) 0.001(3) -0.002(3) -0.003(3) C31 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C32 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C33 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C34 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C35 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C36 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) Si7 0.014(3) 0.015(4) 0.016(4) -0.006(3) -0.003(3) -0.004(3) Si8 0.021(4) 0.014(3) 0.017(4) -0.003(3) -0.011(3) -0.004(3) C19 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C20 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C21 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C22 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C23 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C24 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) Si3 0.032(5) 0.036(5) 0.065(7) -0.001(5) -0.014(5) -0.001(4) Si4 0.040(6) 0.028(5) 0.051(6) -0.002(4) -0.016(5) -0.004(4) C7 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C8 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C9 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C10 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C11 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C12 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) Si5 0.025(5) 0.035(5) 0.055(6) -0.011(4) -0.011(4) -0.010(4) Si6 0.030(5) 0.039(5) 0.041(5) -0.010(4) -0.012(4) -0.007(4) C13 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C14 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C15 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C16 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C17 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C18 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) Si9 0.026(5) 0.046(6) 0.036(5) -0.005(4) -0.008(4) -0.013(4) Si10 0.024(5) 0.046(6) 0.041(5) -0.008(4) -0.006(4) -0.014(4) C25 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C26 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C27 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C28 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C29 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C30 0.035(3) 0.037(3) 0.041(3) -0.004(2) -0.010(2) -0.010(2) C55 0.031(11) 0.054(13) 0.110(19) 0.045(13) 0.002(11) 0.007(10) C54 0.032(9) 0.039(10) 0.055(12) 0.001(8) -0.007(8) -0.005(8) C53 0.014(7) 0.032(9) 0.040(9) 0.001(7) -0.005(6) 0.001(6) C52 0.030(9) 0.035(9) 0.029(8) -0.008(7) -0.007(7) -0.006(7) C51 0.034(9) 0.054(11) 0.028(9) -0.009(8) 0.001(7) -0.001(8) C50 0.066(15) 0.070(15) 0.065(15) 0.053(12) 0.004(12) 0.005(12) K002 0.031(3) 0.031(3) 0.038(3) 0.002(2) -0.007(2) -0.003(2) N1 0.022(8) 0.024(9) 0.020(8) 0.006(7) -0.019(7) -0.010(7) N2 0.023(6) 0.010(6) 0.046(8) 0.001(5) -0.022(6) 0.000(5) N3 0.017(6) 0.026(6) 0.034(7) -0.016(5) -0.011(5) -0.006(5) N4 0.022(6) 0.043(8) 0.022(6) -0.004(5) -0.010(5) -0.011(6) O3 0.022(5) 0.031(6) 0.035(6) 0.000(5) -0.008(5) -0.005(5) O1 0.113(13) 0.063(9) 0.067(10) -0.005(8) -0.034(9) -0.042(9) O2 0.035(6) 0.050(7) 0.025(6) 0.013(5) -0.001(5) -0.001(6) O4 0.030(6) 0.031(6) 0.056(8) 0.009(5) 0.002(6) -0.003(5) Th01 0.0152(2) 0.0163(2) 0.0193(2) -0.00200(17) -0.00638(17) -0.00381(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 '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' 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 N2 Si1 C3 108.5(9) . . N2 Si1 C1 111.1(10) . . C3 Si1 C1 105.8(5) . . N2 Si1 C2 119.8(10) . . C3 Si1 C2 105.4(5) . . C1 Si1 C2 105.3(5) . . N2 Si1 Th01 38.9(3) . . C3 Si1 Th01 71.1(9) . . C1 Si1 Th01 132.8(8) . . C2 Si1 Th01 121.1(8) . . N2 Si2 C6 106.9(10) . . N2 Si2 C4 113.9(10) . . C6 Si2 C4 106.0(5) . . N2 Si2 C5 117.6(10) . . C6 Si2 C5 106.0(5) . . C4 Si2 C5 105.7(5) . . Si1 C1 H1A 109.5 . . Si1 C1 H1B 109.5 . . H1A C1 H1B 109.5 . . Si1 C1 H1C 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . Si1 C2 H2A 109.5 . . Si1 C2 H2B 109.5 . . H2A C2 H2B 109.5 . . Si1 C2 H2C 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . Si1 C3 H3A 109.5 . . Si1 C3 H3B 109.5 . . H3A C3 H3B 109.5 . . Si1 C3 H3C 109.5 . . H3A C3 H3C 109.5 . . H3B C3 H3C 109.5 . . Si2 C4 H4A 109.5 . . Si2 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . Si2 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . Si2 C5 H5A 109.5 . . Si2 C5 H5B 109.5 . . H5A C5 H5B 109.5 . . Si2 C5 H5C 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . Si2 C6 H6A 109.5 . . Si2 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . Si2 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . N4 Si11 C33 111.3(10) . . N4 Si11 C32 110.6(10) . . C33 Si11 C32 106.3(5) . . N4 Si11 C31 116.7(10) . . C33 Si11 C31 105.7(5) . . C32 Si11 C31 105.6(5) . . N4 Si12 C34 114.2(9) . . N4 Si12 C35 109.6(9) . . C34 Si12 C35 105.7(5) . . N4 Si12 C36 116.0(10) . . C34 Si12 C36 105.3(5) . . C35 Si12 C36 105.2(5) . . Si11 C31 H31A 109.5 . . Si11 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . Si11 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . Si11 C32 H32A 109.5 . . Si11 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . Si11 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . Si11 C33 H33A 109.5 . . Si11 C33 H33B 109.5 . . H33A C33 H33B 109.5 . . Si11 C33 H33C 109.5 . . H33A C33 H33C 109.5 . . H33B C33 H33C 109.5 . . Si12 C34 H34A 109.5 . . Si12 C34 H34B 109.5 . . H34A C34 H34B 109.5 . . Si12 C34 H34C 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . Si12 C35 H35A 109.5 . . Si12 C35 H35B 109.5 . . H35A C35 H35B 109.5 . . Si12 C35 H35C 109.5 . . H35A C35 H35C 109.5 . . H35B C35 H35C 109.5 . . Si12 C36 H36A 109.5 . . Si12 C36 H36B 109.5 . . H36A C36 H36B 109.5 . . Si12 C36 H36C 109.5 . . H36A C36 H36C 109.5 . . H36B C36 H36C 109.5 . . N3 Si7 C20 108.9(9) . . N3 Si7 C21 115.8(10) . . C20 Si7 C21 105.8(5) . . N3 Si7 C19 113.9(9) . . C20 Si7 C19 105.9(5) . . C21 Si7 C19 105.8(5) . . N3 Si8 C23 111.6(10) . . N3 Si8 C24 111.8(10) . . C23 Si8 C24 105.9(5) . . N3 Si8 C22 115.8(10) . . C23 Si8 C22 105.5(5) . . C24 Si8 C22 105.5(5) . . Si7 C19 H19A 109.5 . . Si7 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . Si7 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . Si7 C20 H20A 109.5 . . Si7 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . Si7 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . Si7 C21 H21A 109.5 . . Si7 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . Si7 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . Si8 C22 H22A 109.5 . . Si8 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . Si8 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . Si8 C23 H23A 109.5 . . Si8 C23 H23B 109.5 . . H23A C23 H23B 109.5 . . Si8 C23 H23C 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . Si8 C24 H24A 109.5 . . Si8 C24 H24B 109.5 . . H24A C24 H24B 109.5 . . Si8 C24 H24C 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . N2 Si3 C7 111.1(10) . . N2 Si3 C8 111.2(10) . . C7 Si3 C8 106.2(5) . . N2 Si3 C9 116.1(10) . . C7 Si3 C9 105.7(5) . . C8 Si3 C9 105.9(5) . . N2 Si4 C11 109.4(10) . . N2 Si4 C12 116.6(10) . . C11 Si4 C12 105.6(5) . . N2 Si4 C10 113.3(10) . . C11 Si4 C10 105.7(5) . . C12 Si4 C10 105.5(5) . . Si3 C7 H7A 109.5 . . Si3 C7 H7B 109.5 . . H7A C7 H7B 109.5 . . Si3 C7 H7C 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . Si3 C8 H8A 109.5 . . Si3 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . Si3 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . Si3 C9 H9A 109.5 . . Si3 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . Si3 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . Si4 C10 H10A 109.5 . . Si4 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . Si4 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . Si4 C11 H11A 109.5 . . Si4 C11 H11B 109.5 . . H11A C11 H11B 109.5 . . Si4 C11 H11C 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . Si4 C12 H12A 109.5 . . Si4 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . Si4 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . N3 Si5 C15 114.4(10) . . N3 Si5 C13 110.1(10) . . C15 Si5 C13 105.5(5) . . N3 Si5 C14 115.2(10) . . C15 Si5 C14 105.5(5) . . C13 Si5 C14 105.3(5) . . N3 Si6 C16 108.2(10) . . N3 Si6 C18 117.0(10) . . C16 Si6 C18 105.8(5) . . N3 Si6 C17 113.5(10) . . C16 Si6 C17 105.9(5) . . C18 Si6 C17 105.7(5) . . Si5 C13 H13A 109.5 . . Si5 C13 H13B 109.5 . . H13A C13 H13B 109.5 . . Si5 C13 H13C 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . Si5 C14 H14A 109.5 . . Si5 C14 H14B 109.5 . . H14A C14 H14B 109.5 . . Si5 C14 H14C 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . Si5 C15 H15A 109.5 . . Si5 C15 H15B 109.5 . . H15A C15 H15B 109.5 . . Si5 C15 H15C 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . Si6 C16 H16A 109.5 . . Si6 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . Si6 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . Si6 C17 H17A 109.5 . . Si6 C17 H17B 109.5 . . H17A C17 H17B 109.5 . . Si6 C17 H17C 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . Si6 C18 H18A 109.5 . . Si6 C18 H18B 109.5 . . H18A C18 H18B 109.5 . . Si6 C18 H18C 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . N4 Si9 C27 107.6(10) . . N4 Si9 C26 116.4(10) . . C27 Si9 C26 106.1(5) . . N4 Si9 C25 114.2(10) . . C27 Si9 C25 106.1(5) . . C26 Si9 C25 105.8(5) . . N4 Si10 C30 109.5(10) . . N4 Si10 C28 110.4(10) . . C30 Si10 C28 105.5(5) . . N4 Si10 C29 119.9(10) . . C30 Si10 C29 105.3(5) . . C28 Si10 C29 105.1(5) . . N4 Si10 Th01 39.3(3) . . C30 Si10 Th01 71.9(9) . . C28 Si10 Th01 132.6(8) . . C29 Si10 Th01 121.5(8) . . Si9 C25 H25A 109.5 . . Si9 C25 H25B 109.5 . . H25A C25 H25B 109.5 . . Si9 C25 H25C 109.5 . . H25A C25 H25C 109.5 . . H25B C25 H25C 109.5 . . Si9 C26 H26A 109.5 . . Si9 C26 H26B 109.5 . . H26A C26 H26B 109.5 . . Si9 C26 H26C 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . Si9 C27 H27A 109.5 . . Si9 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . Si9 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . Si10 C28 H28A 109.5 . . Si10 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . Si10 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . Si10 C29 H29A 109.5 . . Si10 C29 H29B 109.5 . . H29A C29 H29B 109.5 . . Si10 C29 H29C 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . Si10 C30 H30A 109.5 . . Si10 C30 H30B 109.5 . . H30A C30 H30B 109.5 . . Si10 C30 H30C 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . O1 C59 C58 107(2) . . O1 C59 H59A 110.2 . . C58 C59 H59A 110.2 . . O1 C59 H59B 110.2 . . C58 C59 H59B 110.2 . . H59A C59 H59B 108.5 . . C59 C58 C57 99(3) . . C59 C58 H58A 111.9 . . C57 C58 H58A 111.9 . . C59 C58 H58B 111.9 . . C57 C58 H58B 111.9 . . H58A C58 H58B 109.6 . . C58 C57 C56 112(3) . . C58 C57 H57A 109.2 . . C56 C57 H57A 109.2 . . C58 C57 H57B 109.2 . . C56 C57 H57B 109.2 . . H57A C57 H57B 107.9 . . C60 C61 C62 116(3) . . C60 C61 C56 49.5(14) . . C62 C61 C56 71(2) . . C60 C61 H61A 108.3 . . C62 C61 H61A 108.3 . . C56 C61 H61A 104.7 . . C60 C61 H61B 108.3 . . C62 C61 H61B 108.3 . . C56 C61 H61B 145.9 . . H61A C61 H61B 107.4 . . O1 C62 C61 104(3) . . O1 C62 H62A 111.0 . . C61 C62 H62A 111.0 . . O1 C62 H62B 111.0 . . C61 C62 H62B 111.0 . . H62A C62 H62B 109.0 . . C56 C60 C61 81(3) . . C56 C60 H60A 115.1 . . C61 C60 H60A 115.1 . . C56 C60 H60B 115.1 . . C61 C60 H60B 115.1 . . H60A C60 H60B 112.2 . . O4 C55 C50 108.6(17) . 2_676 O4 C55 H55A 110.0 . . C50 C55 H55A 110.0 2_676 . O4 C55 H55B 110.0 . . C50 C55 H55B 110.0 2_676 . H55A C55 H55B 108.4 . . O4 C54 C53 111.8(14) . . O4 C54 H54A 109.3 . . C53 C54 H54A 109.3 . . O4 C54 H54B 109.3 . . C53 C54 H54B 109.3 . . H54A C54 H54B 107.9 . . O3 C53 C54 110.4(13) . . O3 C53 H53A 109.6 . . C54 C53 H53A 109.6 . . O3 C53 H53B 109.6 . . C54 C53 H53B 109.6 . . H53A C53 H53B 108.1 . . O3 C52 C51 108.0(13) . . O3 C52 H52A 110.1 . . C51 C52 H52A 110.1 . . O3 C52 H52B 110.1 . . C51 C52 H52B 110.1 . . H52A C52 H52B 108.4 . . O2 C51 C52 111.0(13) . . O2 C51 H51A 109.4 . . C52 C51 H51A 109.4 . . O2 C51 H51B 109.4 . . C52 C51 H51B 109.4 . . H51A C51 H51B 108.0 . . O2 C50 C55 110.1(18) . 2_676 O2 C50 H50A 109.6 . . C55 C50 H50A 109.6 2_676 . O2 C50 H50B 109.6 . . C55 C50 H50B 109.6 2_676 . H50A C50 H50B 108.2 . . O1 C56 C60 134(2) . . O1 C56 C57 96(3) . . O1 C56 C61 84.6(15) . . C60 C56 C61 49.5(14) . . O1 C56 H56A 112.5 . . C57 C56 H56A 112.5 . . O1 C56 H56B 112.5 . . C57 C56 H56B 112.5 . . H56A C56 H56B 110.0 . . O1 K002 O1 180.0 . 2_676 O1 K002 O4 101.2(4) . . O1 K002 O4 78.8(4) 2_676 . O1 K002 O4 78.8(4) . 2_676 O1 K002 O4 101.2(4) 2_676 2_676 O4 K002 O4 180.0 . 2_676 O1 K002 O2 100.8(4) . . O1 K002 O2 79.2(4) 2_676 . O4 K002 O2 119.6(3) . . O4 K002 O2 60.4(3) 2_676 . O1 K002 O2 79.2(4) . 2_676 O1 K002 O2 100.8(4) 2_676 2_676 O4 K002 O2 60.4(3) . 2_676 O4 K002 O2 119.6(3) 2_676 2_676 O2 K002 O2 180.0 . 2_676 O1 K002 O3 80.8(4) . 2_676 O1 K002 O3 99.2(4) 2_676 2_676 O4 K002 O3 119.4(3) . 2_676 O4 K002 O3 60.6(3) 2_676 2_676 O2 K002 O3 119.3(3) . 2_676 O2 K002 O3 60.7(3) 2_676 2_676 O1 K002 O3 99.2(4) . . O1 K002 O3 80.8(4) 2_676 . O4 K002 O3 60.6(3) . . O4 K002 O3 119.4(3) 2_676 . O2 K002 O3 60.7(3) . . O2 K002 O3 119.3(3) 2_676 . O3 K002 O3 180.0 2_676 . Th01 N1 Th01 180.00(2) 2_567 . Si2 N2 Si1 117.8(6) . . Si3 N2 Si4 115.3(6) . . Si3 N2 Th01 125.2(5) . . Si2 N2 Th01 125.5(4) . . Si1 N2 Th01 114.1(4) . . Si4 N2 Th01 119.0(5) . . Si8 N3 Si7 116.8(6) . . Si5 N3 Si6 116.2(6) . . Si8 N3 Th01 126.8(4) . . Si5 N3 Th01 127.1(5) . . Si7 N3 Th01 116.3(4) . . Si6 N3 Th01 116.6(4) . . Si9 N4 Si10 118.0(6) . . Si11 N4 Si12 116.4(6) . . Si11 N4 Th01 124.7(5) . . Si9 N4 Th01 125.5(5) . . Si10 N4 Th01 113.4(5) . . Si12 N4 Th01 118.6(4) . . C53 O3 C52 112.5(11) . . C53 O3 K002 112.8(8) . . C52 O3 K002 113.6(8) . . C56 O1 C62 92(2) . . C56 O1 C59 111(2) . . C56 O1 K002 127.1(13) . . C62 O1 K002 137(2) . . C59 O1 K002 121.8(18) . . C51 O2 C50 112.8(14) . . C51 O2 K002 112.5(9) . . C50 O2 K002 114.7(11) . . C55 O4 C54 113.1(14) . . C55 O4 K002 116.0(10) . . C54 O4 K002 112.7(9) . . N1 Th01 N3 110.82(18) . . N1 Th01 N4 109.25(18) . . N3 Th01 N4 107.9(2) . . N1 Th01 N2 109.07(19) . . N3 Th01 N2 108.1(2) . . N4 Th01 N2 111.7(2) . . N1 Th01 Si10 95.45(15) . . N3 Th01 Si10 135.1(2) . . N4 Th01 Si10 27.29(18) . . N2 Th01 Si10 95.9(2) . . N1 Th01 Si1 95.17(11) . . N3 Th01 Si1 135.0(2) . . N4 Th01 Si1 96.39(19) . . N2 Th01 Si1 26.94(16) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 N2 1.739(7) . Si1 C3 1.868(8) . Si1 C1 1.869(8) . Si1 C2 1.874(8) . Si1 Th01 3.503(6) . Si2 N2 1.718(7) . Si2 C6 1.866(8) . Si2 C4 1.866(8) . Si2 C5 1.867(8) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 0.9800 . C3 H3A 0.9800 . C3 H3B 0.9800 . C3 H3C 0.9800 . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 H5C 0.9800 . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 H6C 0.9800 . Si11 N4 1.718(7) . Si11 C33 1.863(8) . Si11 C32 1.867(8) . Si11 C31 1.871(8) . Si12 N4 1.750(7) . Si12 C34 1.870(8) . Si12 C35 1.870(8) . Si12 C36 1.873(8) . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C33 H33A 0.9800 . C33 H33B 0.9800 . C33 H33C 0.9800 . C34 H34A 0.9800 . C34 H34B 0.9800 . C34 H34C 0.9800 . C35 H35A 0.9800 . C35 H35B 0.9800 . C35 H35C 0.9800 . C36 H36A 0.9800 . C36 H36B 0.9800 . C36 H36C 0.9800 . Si7 N3 1.732(7) . Si7 C20 1.867(8) . Si7 C21 1.867(8) . Si7 C19 1.868(8) . Si8 N3 1.718(7) . Si8 C23 1.866(8) . Si8 C24 1.868(8) . Si8 C22 1.872(8) . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C24 H24A 0.9800 . C24 H24B 0.9800 . C24 H24C 0.9800 . Si3 N2 1.716(7) . Si3 C7 1.865(8) . Si3 C8 1.866(8) . Si3 C9 1.868(8) . Si4 N2 1.744(7) . Si4 C11 1.868(8) . Si4 C12 1.869(8) . Si4 C10 1.872(8) . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . Si5 N3 1.722(7) . Si5 C15 1.869(8) . Si5 C13 1.870(8) . Si5 C14 1.872(8) . Si6 N3 1.733(7) . Si6 C16 1.866(8) . Si6 C18 1.868(8) . Si6 C17 1.870(8) . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 0.9800 . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 H14C 0.9800 . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 H15C 0.9800 . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C17 H17A 0.9800 . C17 H17B 0.9800 . C17 H17C 0.9800 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . Si9 N4 1.718(7) . Si9 C27 1.864(8) . Si9 C26 1.867(8) . Si9 C25 1.868(8) . Si10 N4 1.742(7) . Si10 C30 1.871(8) . Si10 C28 1.871(8) . Si10 C29 1.874(8) . Si10 Th01 3.486(8) . C25 H25A 0.9800 . C25 H25B 0.9800 . C25 H25C 0.9800 . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C59 O1 1.44(2) . C59 C58 1.51(2) . C59 H59A 0.9900 . C59 H59B 0.9900 . C58 C57 1.51(2) . C58 H58A 0.9900 . C58 H58B 0.9900 . C57 C56 1.51(2) . C57 H57A 0.9900 . C57 H57B 0.9900 . C61 C60 1.51(2) . C61 C62 1.51(2) . C61 C56 1.96(5) . C61 H61A 0.9900 . C61 H61B 0.9900 . C62 O1 1.44(2) . C62 H62A 0.9900 . C62 H62B 0.9900 . C60 C56 1.51(2) . C60 H60A 0.9900 . C60 H60B 0.9900 . C55 O4 1.41(2) . C55 C50 1.51(3) 2_676 C55 H55A 0.9900 . C55 H55B 0.9900 . C54 O4 1.410(19) . C54 C53 1.44(2) . C54 H54A 0.9900 . C54 H54B 0.9900 . C53 O3 1.385(16) . C53 H53A 0.9900 . C53 H53B 0.9900 . C52 O3 1.403(17) . C52 C51 1.49(2) . C52 H52A 0.9900 . C52 H52B 0.9900 . C51 O2 1.395(18) . C51 H51A 0.9900 . C51 H51B 0.9900 . C50 O2 1.42(2) . C50 C55 1.51(3) 2_676 C50 H50A 0.9900 . C50 H50B 0.9900 . C56 O1 1.43(2) . C56 H56A 0.9900 . C56 H56B 0.9900 . K002 O1 2.746(14) . K002 O1 2.746(14) 2_676 K002 O4 2.796(11) . K002 O4 2.796(11) 2_676 K002 O2 2.800(10) . K002 O2 2.800(10) 2_676 K002 O3 2.815(10) 2_676 K002 O3 2.815(10) . N1 Th01 2.1167(7) 2_567 N1 Th01 2.1167(7) . N2 Th01 2.412(8) . N3 Th01 2.399(8) . N4 Th01 2.406(9) .