#------------------------------------------------------------------------------ #$Date: 2019-12-09 12:42:06 +0200 (Mon, 09 Dec 2019) $ #$Revision: 244963 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556484.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_1556484 loop_ _publ_author_name 'Feichtner, K.-S.' 'Gessner, V.H.' _publ_section_title ; Synthesis and Characterization of a Sulfonyl- and Iminophosphoryl-Functionalized Methanide and Methandiide ; _journal_name_full Inorganics _journal_page_first 40 _journal_paper_doi 10.3390/inorganics4040040 _journal_volume 4 _journal_year 2016 _chemical_formula_sum 'C48 H58 K2 N2 O5 P2 S2 Si2' _chemical_formula_weight 1003.40 _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 mixed _cell_angle_alpha 112.315(3) _cell_angle_beta 90.340(3) _cell_angle_gamma 110.779(3) _cell_formula_units_Z 2 _cell_length_a 11.2841(10) _cell_length_b 15.3705(14) _cell_length_c 16.8163(15) _cell_measurement_reflns_used 7525 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.998 _cell_measurement_theta_min 1.956 _cell_volume 2489.2(4) _computing_cell_refinement 'Saint+ ver. 7.68A (Bruker AXS)' _computing_data_collection 'APEX2 ver. 2014.9 (Bruker AXS)' _computing_data_reduction 'Saint+ ver. 7.68A (Bruker AXS)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-CCD' _diffrn_measurement_method omega-scans _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_unetI/netI 0.0611 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 37279 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 1.956 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6528 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details Sadabs2008 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_description needle _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.487 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.064 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 605 _refine_ls_number_reflns 8770 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0408 _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^)+(0.0465P)^2^+1.1645P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.1028 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6524 _reflns_number_total 8770 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Inorganics-2016-4-40.cif _cod_data_source_block platon_pl _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Empirical' was changed to 'empirical' in accordance with the built-in table derived from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated on 2014-11-21. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 1556484 _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_res_file ; platon_pl.res created by SHELXL-2014/7 TITL sad in P1 New: P-1 CELL 0.71073 11.2841 15.3705 16.8163 112.315 90.340 110.779 ZERR 2 0.0010 0.0014 0.0015 0.003 0.003 0.003 LATT 1 SFAC C H K N O P S Si UNIT 96 116 4 4 10 4 4 4 TEMP -173 L.S. 5 OMIt -3 50 OMIT 0 0 1 FMAP 2 PLAN -20 ACTA BOND $H CONF WGHT 0.046500 1.164500 FVAR 0.13570 RESI 0 K1 3 0.301622 0.575791 0.282122 11.00000 0.02483 0.02776 = 0.02071 0.01039 0.00537 0.01793 H1 2 -0.065676 0.653444 0.207718 11.00000 0.01538 O1 5 -0.107211 0.463755 0.087539 11.00000 0.02644 0.02279 = 0.01801 0.00854 -0.00216 0.00829 SI1 8 0.239976 0.803530 0.459667 11.00000 0.02081 0.02131 = 0.01964 0.00785 0.00282 0.01097 N1 4 0.210305 0.735632 0.350543 11.00000 0.02268 0.02011 = 0.02160 0.01000 0.00590 0.01320 P1 6 0.143982 0.741324 0.271413 11.00000 0.01627 0.01744 = 0.01783 0.00866 0.00530 0.00952 S1 7 -0.014358 0.523328 0.166893 11.00000 0.01627 0.01857 = 0.01575 0.00883 0.00380 0.00823 C1 1 0.002477 0.642952 0.209910 11.00000 0.01365 0.02299 = 0.02310 0.01248 0.00618 0.01025 K2 3 0.228401 0.487067 0.017903 11.00000 0.02146 0.02873 = 0.01746 0.01178 0.00604 0.01577 O2 5 0.112359 0.518705 0.159626 11.00000 0.01859 0.02069 = 0.02181 0.00931 0.00822 0.01181 SI2 8 0.315391 0.372685 0.337458 11.00000 0.02074 0.02223 = 0.01755 0.00957 0.00245 0.00639 N2 4 0.315407 0.384628 0.242012 11.00000 0.01839 0.02237 = 0.02178 0.01183 0.00479 0.01080 P2 6 0.362655 0.334993 0.155445 11.00000 0.01563 0.01674 = 0.01723 0.00800 0.00288 0.00886 S2 7 0.542310 0.525098 0.153981 11.00000 0.01474 0.02040 = 0.01680 0.00913 0.00474 0.00796 C2 1 0.102432 0.852558 0.301871 11.00000 0.01937 0.01700 = 0.01530 0.00710 0.00158 0.00971 C38 1 0.657903 0.766459 0.386009 11.00000 0.01973 0.02270 = 0.03785 -0.00102 0.00609 0.00425 AFIX 43 H38 2 0.654896 0.832299 0.409937 11.00000 -1.20000 AFIX 0 C13 1 0.228471 0.722589 0.110746 11.00000 0.01982 0.01775 = 0.02471 0.00950 0.00654 0.00912 AFIX 43 H13 2 0.140743 0.684261 0.084915 11.00000 -1.20000 AFIX 0 C17 1 -0.165112 0.364519 0.346432 11.00000 0.03553 0.04072 = 0.04373 0.03180 0.01106 0.00917 AFIX 43 H17 2 -0.198184 0.331664 0.383919 11.00000 -1.20000 AFIX 0 C11 1 0.447490 0.798572 0.096200 11.00000 0.02500 0.02950 = 0.03998 0.02253 0.01990 0.01568 AFIX 43 H11 2 0.510872 0.812543 0.060917 11.00000 -1.20000 AFIX 0 C15 1 -0.138239 0.356793 0.203230 11.00000 0.04023 0.02553 = 0.02972 0.01385 0.00218 0.00472 AFIX 43 H15 2 -0.151782 0.318145 0.142117 11.00000 -1.20000 AFIX 0 C14 1 -0.075366 0.460967 0.237215 11.00000 0.01240 0.02570 = 0.02121 0.01476 0.00287 0.00888 C44 1 0.348256 0.500127 0.427566 11.00000 0.04675 0.03056 = 0.02033 0.01106 0.00422 0.00912 H44C 2 0.425544 0.553603 0.423852 11.00000 0.05990 H44B 2 0.358220 0.499066 0.485202 11.00000 0.04463 H44A 2 0.270148 0.518328 0.425084 11.00000 0.01679 C16 1 -0.181794 0.308185 0.257863 11.00000 0.04626 0.02869 = 0.04553 0.02252 0.00859 0.00394 AFIX 43 H16 2 -0.223211 0.236006 0.234462 11.00000 -1.20000 AFIX 0 C40 1 0.716185 0.639194 0.403013 11.00000 0.03256 0.03721 = 0.02376 0.01479 0.00122 0.00601 AFIX 43 H40 2 0.754345 0.617470 0.438466 11.00000 -1.20000 AFIX 0 C39 1 0.712142 0.734839 0.437670 11.00000 0.02558 0.03660 = 0.02060 0.00127 0.00244 -0.00059 AFIX 43 H39 2 0.746731 0.778786 0.497078 11.00000 -1.20000 AFIX 0 C3 1 -0.008228 0.851570 0.338352 11.00000 0.02190 0.02007 = 0.02703 0.00950 0.00621 0.00905 AFIX 43 H3 2 -0.066032 0.790572 0.340845 11.00000 -1.20000 AFIX 0 O3 5 0.425754 0.543276 0.143299 11.00000 0.01857 0.02478 = 0.02076 0.01140 0.00397 0.01205 C4 1 -0.034387 0.938212 0.370768 11.00000 0.02290 0.03005 = 0.03382 0.01093 0.00703 0.01467 AFIX 43 H4 2 -0.110236 0.936784 0.395409 11.00000 -1.20000 AFIX 0 O4 5 0.642276 0.560644 0.107289 11.00000 0.02195 0.02751 = 0.02524 0.01400 0.01094 0.00977 C5 1 0.049113 1.027364 0.367682 11.00000 0.03270 0.02282 = 0.02829 0.00626 0.00444 0.01844 AFIX 43 H5 2 0.031212 1.087342 0.390633 11.00000 -1.20000 AFIX 0 C6 1 0.158049 1.029036 0.331347 11.00000 0.03310 0.01990 = 0.02831 0.01063 0.00474 0.01032 AFIX 43 H6 2 0.215203 1.090157 0.328716 11.00000 -1.20000 AFIX 0 C7 1 0.184872 0.942280 0.298625 11.00000 0.02251 0.02235 = 0.02177 0.01067 0.00538 0.01147 AFIX 43 H7 2 0.260547 0.944112 0.273652 11.00000 -1.20000 AFIX 0 C8 1 0.262745 0.759756 0.200060 11.00000 0.01637 0.01388 = 0.02622 0.00996 0.00682 0.00910 C9 1 0.390755 0.816159 0.236463 11.00000 0.02243 0.02421 = 0.02789 0.01403 0.00354 0.00943 AFIX 43 H9 2 0.415835 0.841337 0.297565 11.00000 -1.20000 AFIX 0 C10 1 0.482481 0.836262 0.184951 11.00000 0.01662 0.03420 = 0.04468 0.02305 0.00762 0.01106 AFIX 43 H10 2 0.569954 0.876199 0.210816 11.00000 -1.20000 AFIX 0 C12 1 0.321010 0.740735 0.058446 11.00000 0.02912 0.02666 = 0.02384 0.01329 0.01089 0.01301 AFIX 43 H12 2 0.297035 0.713366 -0.002959 11.00000 -1.20000 AFIX 0 C21 1 0.295766 0.944510 0.496427 11.00000 0.04404 0.02564 = 0.02731 0.00490 -0.00617 0.01374 AFIX 137 H21A 2 0.319145 0.977643 0.560023 11.00000 -1.50000 H21B 2 0.226628 0.961098 0.478565 11.00000 -1.50000 H21C 2 0.370816 0.968805 0.469992 11.00000 -1.50000 AFIX 0 C20 1 0.095777 0.764903 0.511422 11.00000 0.03305 0.04363 = 0.02340 0.01150 0.00988 0.01984 AFIX 137 H20A 2 0.117020 0.806215 0.574394 11.00000 -1.50000 H20B 2 0.068816 0.692714 0.500235 11.00000 -1.50000 H20C 2 0.025758 0.775492 0.486821 11.00000 -1.50000 AFIX 0 C19 1 -0.055284 0.516751 0.325400 11.00000 0.04112 0.02561 = 0.02620 0.01401 0.00620 0.00826 AFIX 43 H19 2 -0.010412 0.588647 0.349145 11.00000 -1.20000 AFIX 0 C18 1 -0.100752 0.467764 0.379734 11.00000 0.05270 0.03710 = 0.02317 0.01768 0.00879 0.01173 AFIX 43 H18 2 -0.086975 0.506471 0.440848 11.00000 -1.20000 AFIX 0 C22 1 0.369541 0.781261 0.508167 11.00000 0.03076 0.03922 = 0.02761 0.01596 0.00187 0.01930 AFIX 137 H22A 2 0.387324 0.820440 0.571447 11.00000 -1.50000 H22B 2 0.447589 0.803115 0.483521 11.00000 -1.50000 H22C 2 0.341847 0.708516 0.495038 11.00000 -1.50000 AFIX 0 C32 1 0.172492 0.241273 -0.088279 11.00000 0.03107 0.02004 = 0.02043 0.00840 0.00059 0.00929 H32 2 0.196107 0.229701 -0.148257 11.00000 0.02690 C31 1 0.268534 0.278665 -0.018365 11.00000 0.02129 0.01775 = 0.02228 0.01019 0.00332 0.00870 H31 2 0.357181 0.295916 -0.022756 11.00000 0.01339 C30 1 0.238646 0.294718 0.064721 11.00000 0.01898 0.01609 = 0.01875 0.00703 0.00093 0.00828 C29 1 0.261333 0.136061 0.136119 11.00000 0.03029 0.02257 = 0.02642 0.01104 0.00254 0.01176 AFIX 43 H29 2 0.181780 0.143874 0.133409 11.00000 -1.20000 AFIX 0 C28 1 0.262550 0.046139 0.134644 11.00000 0.04299 0.02121 = 0.03651 0.01354 0.00247 0.01008 AFIX 43 H28 2 0.184424 -0.007726 0.130186 11.00000 -1.20000 AFIX 0 C27 1 0.377415 0.034868 0.139657 11.00000 0.05873 0.03164 = 0.05249 0.02278 0.00874 0.02798 AFIX 43 H27 2 0.378855 -0.026837 0.138967 11.00000 -1.20000 AFIX 0 C26 1 0.488995 0.111809 0.145601 11.00000 0.04653 0.05135 = 0.06666 0.03267 0.01652 0.03665 AFIX 43 H26 2 0.568252 0.103895 0.149773 11.00000 -1.20000 AFIX 0 C25 1 0.488083 0.201692 0.145626 11.00000 0.02864 0.03731 = 0.05472 0.02665 0.00865 0.01755 AFIX 43 H25 2 0.566524 0.254367 0.148513 11.00000 -1.20000 AFIX 0 C24 1 0.373734 0.215340 0.141474 11.00000 0.02476 0.02109 = 0.02262 0.00884 0.00359 0.01231 C23 1 0.507263 0.405353 0.135384 11.00000 0.01446 0.02316 = 0.01859 0.00575 0.00356 0.01133 H23 2 0.557988 0.380508 0.121110 11.00000 0.04148 C33 1 0.046125 0.219386 -0.075876 11.00000 0.02561 0.02255 = 0.02573 0.01032 -0.00654 0.00577 AFIX 43 H33 2 -0.019894 0.192412 -0.124083 11.00000 -1.20000 AFIX 0 C34 1 0.015987 0.236766 0.006613 11.00000 0.01726 0.03078 = 0.02929 0.01476 0.00002 0.00668 AFIX 43 H34 2 -0.070788 0.222746 0.015307 11.00000 -1.20000 AFIX 0 C35 1 0.111597 0.274547 0.076799 11.00000 0.02074 0.02165 = 0.02130 0.01108 0.00415 0.00778 AFIX 43 H35 2 0.090232 0.286751 0.133535 11.00000 -1.20000 AFIX 0 C36 1 0.609705 0.606746 0.265847 11.00000 0.01065 0.01965 = 0.02009 0.00698 0.00352 0.00303 C37 1 0.608400 0.703828 0.300611 11.00000 0.01960 0.02645 = 0.03066 0.00966 0.00417 0.00828 H37 2 0.578188 0.723791 0.264284 11.00000 0.02482 C41 1 0.664951 0.574959 0.316977 11.00000 0.02410 0.02507 = 0.02168 0.01117 0.00180 0.00606 AFIX 43 H41 2 0.667774 0.509057 0.293101 11.00000 -1.20000 AFIX 0 C42 1 0.435470 0.324245 0.361218 11.00000 0.03207 0.04040 = 0.03058 0.01998 -0.00135 0.01337 AFIX 137 H42A 2 0.433944 0.325561 0.419918 11.00000 -1.50000 H42B 2 0.521404 0.367599 0.357661 11.00000 -1.50000 H42C 2 0.414096 0.254147 0.318546 11.00000 -1.50000 AFIX 0 C43 1 0.155330 0.288187 0.345587 11.00000 0.02509 0.03206 = 0.02726 0.01562 0.00645 0.00824 AFIX 137 H43A 2 0.137771 0.217608 0.305582 11.00000 -1.50000 H43B 2 0.089321 0.309249 0.330088 11.00000 -1.50000 H43C 2 0.154339 0.293065 0.405384 11.00000 -1.50000 AFIX 0 RESI 1 O1 5 0.716850 0.031439 0.165182 11.00000 0.03440 0.05855 = 0.04194 0.02895 0.01022 0.02534 C2 1 0.873651 0.006930 0.075447 11.00000 0.02868 0.03368 = 0.05157 0.01576 0.00910 0.01049 AFIX 23 H2A 2 0.860023 -0.066142 0.049230 11.00000 -1.20000 H2B 2 0.927163 0.041502 0.041484 11.00000 -1.20000 AFIX 0 C3 1 0.932882 0.055646 0.168136 11.00000 0.03331 0.05946 = 0.05442 0.01255 -0.00090 0.01660 AFIX 23 H3A 2 0.978930 0.130144 0.187449 11.00000 -1.20000 H3B 2 0.993746 0.026394 0.178387 11.00000 -1.20000 AFIX 0 C4 1 0.821423 0.032268 0.214092 11.00000 0.03492 0.06153 = 0.04890 0.02654 -0.00470 0.01451 AFIX 23 H4A 2 0.800484 -0.034919 0.216323 11.00000 -1.20000 H4B 2 0.840691 0.084919 0.274405 11.00000 -1.20000 AFIX 0 C1 1 0.746393 0.020681 0.079906 11.00000 0.03743 0.05233 = 0.04075 0.02162 0.01118 0.02115 AFIX 23 H1A 2 0.753899 0.082148 0.070590 11.00000 -1.20000 H1B 2 0.678006 -0.039299 0.034647 11.00000 -1.20000 REM ##### REM ##### RESI 0 AFIX 0 HKLF 4 REM sad in P1 New: P-1 REM R1 = 0.0408 for 6524 Fo > 4sig(Fo) and 0.0662 for all 8770 data REM 605 parameters refined using 0 restraints END WGHT 0.0390 1.4692 REM Highest difference peak 0.487, deepest hole -0.378, 1-sigma level 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10.75 6 -6 0 34.82 1.77 6 -6 0 36.91 2.10 6 -6 0 46.18 10.19 6 -6 0 39.48 2.28 -6 6 0 38.78 2.06 -6 6 0 37.53 1.69 -6 6 0 48.60 10.48 -6 6 0 18.17 7.19 5 -6 0 -0.08 0.73 5 -6 0 0.40 0.40 5 -6 0 1.33 3.67 5 -6 0 -1.07 4.20 -5 6 0 1.58 4.36 -5 6 0 2.92 4.71 -5 6 0 1.67 0.71 -5 6 0 0.80 0.37 4 -6 0 87.77 3.85 4 -6 0 90.69 3.62 4 -6 0 101.28 12.58 -4 6 0 81.64 11.28 -4 6 0 89.06 3.63 -4 6 0 90.90 3.47 -4 6 0 83.90 11.40 -4 6 0 86.58 3.91 3 -6 0 12.33 4.37 3 -6 0 8.89 4.04 -3 6 0 8.73 0.49 -3 6 0 9.03 0.95 -3 6 0 6.77 3.83 -3 6 0 8.04 0.56 -3 6 0 7.13 3.90 2 -6 0 50.88 2.44 2 -6 0 41.03 5.92 2 -6 0 54.65 2.50 -2 6 0 51.54 2.46 -2 6 0 51.71 2.07 -2 6 0 51.84 2.43 -2 6 0 63.59 7.57 -2 6 0 52.00 2.36 -2 6 0 61.76 7.23 -2 6 0 52.00 2.20 1 -6 0 1.52 2.23 1 -6 0 0.32 0.66 1 -6 0 1.32 1.78 1 -6 0 0.71 0.39 -1 6 0 0.74 0.62 -1 6 0 -0.97 0.56 -1 6 0 1.93 1.96 -1 6 0 0.37 0.38 -1 6 0 1.05 0.54 -1 6 0 4.79 2.42 0 -6 0 11.54 0.83 0 -6 0 8.71 2.15 0 -6 0 11.12 1.10 0 -6 0 8.82 2.52 0 6 0 11.20 0.86 0 6 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14.27 2.03 -4 -8 19 13.90 1.72 3 8 -19 -2.24 1.18 2 8 -19 17.47 2.12 1 8 -19 34.68 2.60 0 8 -19 2.93 1.42 0 -8 19 3.54 1.29 -1 8 -19 -0.26 1.14 1 -8 19 0.08 1.10 -2 8 -19 12.59 1.87 2 -8 19 11.83 1.67 -3 8 -19 2.44 1.43 3 -8 19 0.69 1.09 -4 8 -19 1.58 1.37 -4 8 -19 3.37 1.31 4 -8 19 2.77 1.27 4 7 -19 1.29 1.35 -4 -7 19 0.80 1.11 3 7 -19 16.97 2.04 -3 -7 19 18.86 1.96 2 7 -19 12.95 1.85 -2 -7 19 11.00 1.56 1 7 -19 12.38 1.81 -1 -7 19 14.14 1.65 0 7 -19 1.16 1.35 -1 7 -19 1.83 1.34 1 -7 19 -0.69 1.14 -2 7 -19 32.28 2.56 2 -7 19 28.08 2.22 -3 7 -19 1.20 1.42 -3 7 -19 4.53 1.39 3 -7 19 4.05 1.20 -4 7 -19 -0.41 1.14 -4 7 -19 1.54 1.50 4 -7 19 -0.65 1.04 4 6 -19 0.50 1.36 -4 -6 19 1.85 1.19 3 6 -19 6.65 1.52 -3 -6 19 3.32 1.22 2 6 -19 5.29 1.46 -2 -6 19 6.49 1.34 1 6 -19 2.45 1.32 -1 -6 19 1.56 1.12 0 6 -19 13.39 1.92 0 -6 19 16.11 1.75 -1 6 -19 1.12 1.32 1 -6 19 2.66 1.12 -2 6 -19 4.58 1.42 -2 6 -19 3.76 1.47 2 -6 19 5.08 1.30 -3 6 -19 6.57 1.51 -3 6 -19 7.99 1.75 3 -6 19 10.46 1.61 -4 6 -19 0.15 1.40 -4 6 -19 2.08 1.32 4 -6 19 -0.14 1.12 4 5 -19 4.11 1.41 -4 -5 19 0.55 1.08 3 5 -19 3.86 1.43 -3 -5 19 4.93 1.27 2 5 -19 0.44 1.26 -2 -5 19 -0.39 1.02 1 5 -19 3.63 1.34 -1 -5 19 2.49 1.15 0 5 -19 11.59 1.82 0 -5 19 15.88 1.69 -1 5 -19 7.14 1.59 1 -5 19 2.88 1.18 -2 5 -19 1.26 1.33 -2 5 -19 4.98 1.36 -3 5 -19 23.22 2.19 -3 5 -19 20.80 2.37 3 -5 19 19.35 1.97 4 4 -19 -0.11 1.22 -4 -4 19 1.69 1.13 3 4 -19 8.60 1.65 -3 -4 19 6.83 1.32 2 4 -19 6.84 1.57 -2 -4 19 4.09 1.24 1 4 -19 5.50 1.52 -1 -4 19 3.23 1.20 0 4 -19 3.11 1.38 0 -4 19 1.63 1.06 -1 4 -19 1.74 1.23 -1 4 -19 2.07 1.38 1 -4 19 2.05 1.09 -2 4 -19 -1.28 1.25 -2 4 -19 0.61 1.07 2 -4 19 -2.32 0.98 -3 4 -19 3.47 1.37 -3 4 -19 0.01 1.49 4 3 -19 1.07 1.26 -4 -3 19 2.84 1.25 3 3 -19 2.36 1.38 -3 -3 19 3.71 1.28 2 3 -19 -1.37 1.19 -2 -3 19 -1.03 0.99 1 3 -19 0.08 1.23 -1 -3 19 -0.09 1.04 0 3 -19 -1.44 1.02 0 3 -19 2.36 1.40 0 -3 19 1.30 1.08 -1 3 -19 3.34 1.52 -1 3 -19 2.80 1.29 1 -3 19 2.20 1.10 -2 3 -19 2.38 1.47 -2 3 -19 0.00 1.17 2 -3 19 2.75 1.09 4 2 -19 -0.43 1.25 -4 -2 19 1.11 1.06 3 2 -19 -0.72 1.23 -3 -2 19 1.07 1.16 2 2 -19 1.05 1.28 -2 -2 19 1.01 1.14 1 2 -19 9.99 1.53 1 2 -19 7.51 1.69 -1 -2 19 5.93 1.34 0 2 -19 3.51 1.32 0 2 -19 3.93 1.52 0 -2 19 3.73 1.21 -1 2 -19 4.40 1.41 -1 2 -19 6.74 1.65 1 -2 19 0.44 1.08 3 1 -19 0.61 1.21 -3 -1 19 -1.26 1.10 2 1 -19 1.44 1.16 2 1 -19 4.26 1.46 -2 -1 19 0.27 1.10 1 1 -19 0.85 1.20 1 1 -19 1.34 1.41 -1 -1 19 0.35 1.10 0 1 -19 0.48 1.40 0 1 -19 2.48 1.31 0 -1 19 1.24 1.13 -1 10 -20 5.30 1.61 1 -10 20 4.29 1.40 1 9 -20 0.29 1.30 -1 -9 20 1.00 1.25 0 9 -20 0.91 1.38 0 -9 20 0.18 1.18 -1 9 -20 3.96 1.44 1 -9 20 5.31 1.41 -2 9 -20 -2.24 1.09 2 -9 20 -0.73 1.11 1 8 -20 2.41 1.44 -1 -8 20 3.42 1.27 0 8 -20 0.08 1.30 0 -8 20 -0.42 1.19 -1 8 -20 3.32 1.49 1 -8 20 0.51 1.18 -2 8 -20 3.12 1.46 2 -8 20 5.32 1.39 2 7 -20 2.36 1.38 -2 -7 20 3.61 1.27 1 7 -20 7.15 1.62 -1 -7 20 5.91 1.39 0 7 -20 1.59 1.38 -1 7 -20 0.04 1.23 1 -7 20 -0.62 1.09 -2 7 -20 7.81 1.67 2 -7 20 5.78 1.39 2 6 -20 3.18 1.54 -2 -6 20 5.99 1.31 1 6 -20 8.07 1.66 -1 -6 20 7.87 1.50 0 6 -20 4.01 1.44 0 -6 20 3.50 1.21 -1 6 -20 0.33 1.22 2 5 -20 13.15 1.95 -2 -5 20 7.27 1.47 1 5 -20 4.42 1.49 -1 -5 20 1.01 1.11 0 5 -20 1.92 1.35 0 -5 20 2.30 1.13 -1 5 -20 8.85 1.67 -1 5 -20 11.22 1.92 1 -5 20 12.28 1.61 1 4 -20 -1.29 1.28 -1 -4 20 0.58 1.12 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 55556 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 K1 K 0.30162(6) 0.57579(5) 0.28212(4) 0.02193(15) Uani 1 1 d . . . . . H1 H -0.066(3) 0.653(2) 0.2077(19) 0.015(8) Uiso 1 1 d . . . . . O1 O -0.10721(19) 0.46376(15) 0.08754(12) 0.0227(5) Uani 1 1 d . . . . . Si1 Si 0.23998(8) 0.80353(6) 0.45967(5) 0.01990(18) Uani 1 1 d . . . . . N1 N 0.2103(2) 0.73563(17) 0.35054(15) 0.0195(5) Uani 1 1 d . . . . . P1 P 0.14398(7) 0.74132(5) 0.27141(5) 0.01579(16) Uani 1 1 d . . . . . S1 S -0.01436(7) 0.52333(5) 0.16689(4) 0.01581(16) Uani 1 1 d . . . . . C1 C 0.0025(3) 0.6430(2) 0.20991(19) 0.0179(6) Uani 1 1 d . . . . . K2 K 0.22840(6) 0.48707(5) 0.01790(4) 0.01994(15) Uani 1 1 d . . . . . O2 O 0.11236(18) 0.51871(14) 0.15963(12) 0.0189(4) Uani 1 1 d . . . . . Si2 Si 0.31539(8) 0.37268(6) 0.33746(5) 0.02027(19) Uani 1 1 d . . . . . N2 N 0.3154(2) 0.38463(18) 0.24201(15) 0.0190(5) Uani 1 1 d . . . . . P2 P 0.36265(7) 0.33499(5) 0.15544(5) 0.01540(16) Uani 1 1 d . . . . . S2 S 0.54231(7) 0.52510(5) 0.15398(4) 0.01645(16) Uani 1 1 d . . . . . C2 C 0.1024(3) 0.8526(2) 0.30187(17) 0.0163(6) Uani 1 1 d . . . . . C38 C 0.6579(3) 0.7665(2) 0.3860(2) 0.0323(8) Uani 1 1 d . . . . . H38 H 0.6549 0.8323 0.4099 0.039 Uiso 1 1 calc R U . . . C13 C 0.2285(3) 0.7226(2) 0.11075(19) 0.0199(6) Uani 1 1 d . . . . . H13 H 0.1407 0.6843 0.0849 0.024 Uiso 1 1 calc R U . . . C17 C -0.1651(3) 0.3645(3) 0.3464(2) 0.0369(8) Uani 1 1 d . . . . . H17 H -0.1982 0.3317 0.3839 0.044 Uiso 1 1 calc R U . . . C11 C 0.4475(3) 0.7986(2) 0.0962(2) 0.0272(7) Uani 1 1 d . . . . . H11 H 0.5109 0.8125 0.0609 0.033 Uiso 1 1 calc R U . . . C15 C -0.1382(3) 0.3568(2) 0.2032(2) 0.0334(8) Uani 1 1 d . . . . . H15 H -0.1518 0.3181 0.1421 0.040 Uiso 1 1 calc R U . . . C14 C -0.0754(3) 0.4610(2) 0.23721(18) 0.0176(6) Uani 1 1 d . . . . . C44 C 0.3483(4) 0.5001(3) 0.4276(2) 0.0341(8) Uani 1 1 d . . . . . H44C H 0.426(4) 0.554(3) 0.424(3) 0.060(12) Uiso 1 1 d . . . . . H44B H 0.358(3) 0.499(3) 0.485(2) 0.045(10) Uiso 1 1 d . . . . . H44A H 0.270(3) 0.518(2) 0.4251(18) 0.017(7) Uiso 1 1 d . . . . . C16 C -0.1818(4) 0.3082(3) 0.2579(2) 0.0409(9) Uani 1 1 d . . . . . H16 H -0.2232 0.2360 0.2345 0.049 Uiso 1 1 calc R U . . . C40 C 0.7162(3) 0.6392(3) 0.4030(2) 0.0327(8) Uani 1 1 d . . . . . H40 H 0.7543 0.6175 0.4385 0.039 Uiso 1 1 calc R U . . . C39 C 0.7121(3) 0.7348(3) 0.4377(2) 0.0348(8) Uani 1 1 d . . . . . H39 H 0.7467 0.7788 0.4971 0.042 Uiso 1 1 calc R U . . . C3 C -0.0082(3) 0.8516(2) 0.33835(19) 0.0227(7) Uani 1 1 d . . . . . H3 H -0.0660 0.7906 0.3408 0.027 Uiso 1 1 calc R U . . . O3 O 0.42575(18) 0.54328(15) 0.14330(12) 0.0196(4) Uani 1 1 d . . . . . C4 C -0.0344(3) 0.9382(2) 0.3708(2) 0.0283(7) Uani 1 1 d . . . . . H4 H -0.1102 0.9368 0.3954 0.034 Uiso 1 1 calc R U . . . O4 O 0.64228(19) 0.56064(15) 0.10729(13) 0.0238(5) Uani 1 1 d . . . . . C5 C 0.0491(3) 1.0274(2) 0.3677(2) 0.0270(7) Uani 1 1 d . . . . . H5 H 0.0312 1.0873 0.3906 0.032 Uiso 1 1 calc R U . . . C6 C 0.1580(3) 1.0290(2) 0.3313(2) 0.0268(7) Uani 1 1 d . . . . . H6 H 0.2152 1.0902 0.3287 0.032 Uiso 1 1 calc R U . . . C7 C 0.1849(3) 0.9423(2) 0.29862(18) 0.0208(6) Uani 1 1 d . . . . . H7 H 0.2605 0.9441 0.2737 0.025 Uiso 1 1 calc R U . . . C8 C 0.2627(3) 0.7598(2) 0.20006(19) 0.0173(6) Uani 1 1 d . . . . . C9 C 0.3908(3) 0.8162(2) 0.2365(2) 0.0236(7) Uani 1 1 d . . . . . H9 H 0.4158 0.8413 0.2976 0.028 Uiso 1 1 calc R U . . . C10 C 0.4825(3) 0.8363(2) 0.1850(2) 0.0292(7) Uani 1 1 d . . . . . H10 H 0.5700 0.8762 0.2108 0.035 Uiso 1 1 calc R U . . . C12 C 0.3210(3) 0.7407(2) 0.0584(2) 0.0249(7) Uani 1 1 d . . . . . H12 H 0.2970 0.7134 -0.0030 0.030 Uiso 1 1 calc R U . . . C21 C 0.2958(3) 0.9445(2) 0.4964(2) 0.0342(8) Uani 1 1 d . . . . . H21A H 0.3191 0.9776 0.5600 0.051 Uiso 1 1 calc R U . . . H21B H 0.2266 0.9611 0.4786 0.051 Uiso 1 1 calc R U . . . H21C H 0.3708 0.9688 0.4700 0.051 Uiso 1 1 calc R U . . . C20 C 0.0958(3) 0.7649(3) 0.5114(2) 0.0325(8) Uani 1 1 d . . . . . H20A H 0.1170 0.8062 0.5744 0.049 Uiso 1 1 calc R U . . . H20B H 0.0688 0.6927 0.5002 0.049 Uiso 1 1 calc R U . . . H20C H 0.0258 0.7755 0.4868 0.049 Uiso 1 1 calc R U . . . C19 C -0.0553(3) 0.5168(2) 0.3254(2) 0.0312(8) Uani 1 1 d . . . . . H19 H -0.0104 0.5886 0.3491 0.037 Uiso 1 1 calc R U . . . C18 C -0.1008(4) 0.4678(3) 0.3797(2) 0.0376(9) Uani 1 1 d . . . . . H18 H -0.0870 0.5065 0.4408 0.045 Uiso 1 1 calc R U . . . C22 C 0.3695(3) 0.7813(3) 0.5082(2) 0.0301(7) Uani 1 1 d . . . . . H22A H 0.3873 0.8204 0.5714 0.045 Uiso 1 1 calc R U . . . H22B H 0.4476 0.8031 0.4835 0.045 Uiso 1 1 calc R U . . . H22C H 0.3418 0.7085 0.4950 0.045 Uiso 1 1 calc R U . . . C32 C 0.1725(3) 0.2413(2) -0.0883(2) 0.0240(7) Uani 1 1 d . . . . . H32 H 0.196(3) 0.230(2) -0.148(2) 0.027(8) Uiso 1 1 d . . . . . C31 C 0.2685(3) 0.2787(2) -0.01837(19) 0.0194(6) Uani 1 1 d . . . . . H31 H 0.357(3) 0.296(2) -0.0228(18) 0.013(7) Uiso 1 1 d . . . . . C30 C 0.2386(3) 0.2947(2) 0.06472(18) 0.0175(6) Uani 1 1 d . . . . . C29 C 0.2613(3) 0.1361(2) 0.1361(2) 0.0256(7) Uani 1 1 d . . . . . H29 H 0.1818 0.1439 0.1334 0.031 Uiso 1 1 calc R U . . . C28 C 0.2626(3) 0.0461(2) 0.1346(2) 0.0337(8) Uani 1 1 d . . . . . H28 H 0.1844 -0.0077 0.1302 0.040 Uiso 1 1 calc R U . . . C27 C 0.3774(4) 0.0349(3) 0.1397(3) 0.0426(9) Uani 1 1 d . . . . . H27 H 0.3789 -0.0268 0.1390 0.051 Uiso 1 1 calc R U . . . C26 C 0.4890(4) 0.1118(3) 0.1456(3) 0.0467(10) Uani 1 1 d . . . . . H26 H 0.5683 0.1039 0.1498 0.056 Uiso 1 1 calc R U . . . C25 C 0.4881(3) 0.2017(3) 0.1456(2) 0.0362(8) Uani 1 1 d . . . . . H25 H 0.5665 0.2544 0.1485 0.043 Uiso 1 1 calc R U . . . C24 C 0.3737(3) 0.2153(2) 0.14147(19) 0.0218(7) Uani 1 1 d . . . . . C23 C 0.5073(3) 0.4054(2) 0.13538(19) 0.0184(6) Uani 1 1 d . . . . . H23 H 0.558(4) 0.381(3) 0.121(2) 0.041(11) Uiso 1 1 d . . . . . C33 C 0.0461(3) 0.2194(2) -0.0759(2) 0.0256(7) Uani 1 1 d . . . . . H33 H -0.0199 0.1924 -0.1241 0.031 Uiso 1 1 calc R U . . . C34 C 0.0160(3) 0.2368(2) 0.0066(2) 0.0258(7) Uani 1 1 d . . . . . H34 H -0.0708 0.2227 0.0153 0.031 Uiso 1 1 calc R U . . . C35 C 0.1116(3) 0.2745(2) 0.07680(19) 0.0206(6) Uani 1 1 d . . . . . H35 H 0.0902 0.2868 0.1335 0.025 Uiso 1 1 calc R U . . . C36 C 0.6097(3) 0.6067(2) 0.26585(18) 0.0180(6) Uani 1 1 d . . . . . C37 C 0.6084(3) 0.7038(2) 0.3006(2) 0.0264(7) Uani 1 1 d . . . . . H37 H 0.578(3) 0.724(2) 0.264(2) 0.025(9) Uiso 1 1 d . . . . . C41 C 0.6650(3) 0.5750(2) 0.31698(19) 0.0241(7) Uani 1 1 d . . . . . H41 H 0.6678 0.5091 0.2931 0.029 Uiso 1 1 calc R U . . . C42 C 0.4355(3) 0.3242(3) 0.3612(2) 0.0328(8) Uani 1 1 d . . . . . H42A H 0.4339 0.3256 0.4199 0.049 Uiso 1 1 calc R U . . . H42B H 0.5214 0.3676 0.3577 0.049 Uiso 1 1 calc R U . . . H42C H 0.4141 0.2541 0.3185 0.049 Uiso 1 1 calc R U . . . C43 C 0.1553(3) 0.2882(2) 0.3456(2) 0.0278(7) Uani 1 1 d . . . . . H43A H 0.1378 0.2176 0.3056 0.042 Uiso 1 1 calc R U . . . H43B H 0.0893 0.3092 0.3301 0.042 Uiso 1 1 calc R U . . . H43C H 0.1543 0.2931 0.4054 0.042 Uiso 1 1 calc R U . . . O1_1 O 0.7169(2) 0.03144(19) 0.16518(16) 0.0400(6) Uani 1 1 d . . . . . C2_1 C 0.8737(3) 0.0069(3) 0.0754(2) 0.0390(9) Uani 1 1 d . . . . . H2A_1 H 0.8600 -0.0661 0.0492 0.047 Uiso 1 1 calc R U . . . H2B_1 H 0.9272 0.0415 0.0415 0.047 Uiso 1 1 calc R U . . . C3_1 C 0.9329(4) 0.0556(3) 0.1681(3) 0.0530(11) Uani 1 1 d . . . . . H3A_1 H 0.9789 0.1301 0.1874 0.064 Uiso 1 1 calc R U . . . H3B_1 H 0.9937 0.0264 0.1784 0.064 Uiso 1 1 calc R U . . . C4_1 C 0.8214(4) 0.0323(3) 0.2141(3) 0.0484(10) Uani 1 1 d . . . . . H4A_1 H 0.8005 -0.0349 0.2163 0.058 Uiso 1 1 calc R U . . . H4B_1 H 0.8407 0.0849 0.2744 0.058 Uiso 1 1 calc R U . . . C1_1 C 0.7464(4) 0.0207(3) 0.0799(2) 0.0415(9) Uani 1 1 d . . . . . H1A_1 H 0.7539 0.0821 0.0706 0.050 Uiso 1 1 calc R U . . . H1B_1 H 0.6780 -0.0393 0.0346 0.050 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 K1 0.0248(4) 0.0278(4) 0.0207(3) 0.0104(3) 0.0054(3) 0.0179(3) O1 0.0264(12) 0.0228(11) 0.0180(10) 0.0085(9) -0.0022(9) 0.0083(9) Si1 0.0208(4) 0.0213(4) 0.0196(4) 0.0079(3) 0.0028(3) 0.0110(4) N1 0.0227(14) 0.0201(13) 0.0216(13) 0.0100(11) 0.0059(11) 0.0132(11) P1 0.0163(4) 0.0174(4) 0.0178(4) 0.0087(3) 0.0053(3) 0.0095(3) S1 0.0163(4) 0.0186(4) 0.0157(3) 0.0088(3) 0.0038(3) 0.0082(3) C1 0.0136(15) 0.0230(16) 0.0231(16) 0.0125(13) 0.0062(12) 0.0102(13) K2 0.0215(3) 0.0287(4) 0.0175(3) 0.0118(3) 0.0060(3) 0.0158(3) O2 0.0186(11) 0.0207(10) 0.0218(10) 0.0093(9) 0.0082(8) 0.0118(9) Si2 0.0207(4) 0.0222(4) 0.0175(4) 0.0096(3) 0.0024(3) 0.0064(4) N2 0.0184(13) 0.0224(13) 0.0218(13) 0.0118(11) 0.0048(10) 0.0108(11) P2 0.0156(4) 0.0167(4) 0.0172(4) 0.0080(3) 0.0029(3) 0.0089(3) S2 0.0147(4) 0.0204(4) 0.0168(3) 0.0091(3) 0.0047(3) 0.0080(3) C2 0.0194(15) 0.0170(14) 0.0153(14) 0.0071(12) 0.0016(12) 0.0097(13) C38 0.0197(17) 0.0227(17) 0.0378(19) -0.0010(15) 0.0061(15) 0.0042(14) C13 0.0198(16) 0.0177(15) 0.0247(16) 0.0095(13) 0.0065(13) 0.0091(13) C17 0.036(2) 0.041(2) 0.044(2) 0.0318(18) 0.0111(17) 0.0092(17) C11 0.0250(18) 0.0295(17) 0.0400(19) 0.0225(15) 0.0199(15) 0.0157(15) C15 0.040(2) 0.0255(18) 0.0297(18) 0.0138(15) 0.0022(15) 0.0047(16) C14 0.0124(14) 0.0257(16) 0.0212(15) 0.0148(13) 0.0029(12) 0.0089(13) C44 0.047(2) 0.0306(19) 0.0203(17) 0.0111(15) 0.0042(16) 0.0091(19) C16 0.046(2) 0.0287(19) 0.046(2) 0.0225(17) 0.0086(18) 0.0039(17) C40 0.033(2) 0.037(2) 0.0238(17) 0.0148(15) 0.0012(14) 0.0060(16) C39 0.0256(19) 0.037(2) 0.0206(17) 0.0013(15) 0.0024(14) -0.0006(16) C3 0.0219(16) 0.0201(15) 0.0270(16) 0.0095(13) 0.0062(13) 0.0091(14) O3 0.0186(11) 0.0248(11) 0.0208(10) 0.0114(9) 0.0040(8) 0.0120(9) C4 0.0229(17) 0.0301(18) 0.0338(18) 0.0109(15) 0.0070(14) 0.0147(15) O4 0.0220(11) 0.0275(11) 0.0252(11) 0.0140(10) 0.0109(9) 0.0098(10) C5 0.0327(19) 0.0228(16) 0.0283(17) 0.0063(14) 0.0044(14) 0.0184(15) C6 0.0331(19) 0.0199(16) 0.0283(17) 0.0106(14) 0.0047(14) 0.0103(15) C7 0.0225(16) 0.0224(16) 0.0218(15) 0.0107(13) 0.0054(13) 0.0115(13) C8 0.0164(15) 0.0139(14) 0.0262(16) 0.0100(12) 0.0068(12) 0.0091(12) C9 0.0224(17) 0.0242(16) 0.0279(16) 0.0140(14) 0.0035(13) 0.0094(14) C10 0.0166(16) 0.0342(18) 0.045(2) 0.0231(16) 0.0076(14) 0.0111(15) C12 0.0291(18) 0.0267(16) 0.0238(16) 0.0133(14) 0.0109(14) 0.0130(15) C21 0.044(2) 0.0256(17) 0.0273(18) 0.0049(15) -0.0062(16) 0.0137(17) C20 0.033(2) 0.044(2) 0.0234(17) 0.0115(15) 0.0099(15) 0.0198(17) C19 0.041(2) 0.0256(17) 0.0262(17) 0.0140(14) 0.0062(15) 0.0083(16) C18 0.053(2) 0.037(2) 0.0232(17) 0.0177(16) 0.0088(17) 0.0117(18) C22 0.0308(19) 0.0392(19) 0.0276(17) 0.0160(15) 0.0019(14) 0.0193(16) C32 0.0311(19) 0.0200(16) 0.0204(16) 0.0084(13) 0.0006(14) 0.0093(14) C31 0.0213(17) 0.0177(15) 0.0223(16) 0.0102(13) 0.0033(13) 0.0087(14) C30 0.0190(15) 0.0161(14) 0.0188(14) 0.0070(12) 0.0009(12) 0.0083(13) C29 0.0303(18) 0.0226(16) 0.0264(16) 0.0110(14) 0.0025(14) 0.0118(15) C28 0.043(2) 0.0212(17) 0.0365(19) 0.0135(15) 0.0025(16) 0.0101(16) C27 0.059(3) 0.032(2) 0.052(2) 0.0228(18) 0.009(2) 0.028(2) C26 0.047(2) 0.051(2) 0.067(3) 0.033(2) 0.017(2) 0.037(2) C25 0.0286(19) 0.037(2) 0.055(2) 0.0267(18) 0.0087(17) 0.0176(17) C24 0.0248(17) 0.0211(16) 0.0226(15) 0.0088(13) 0.0036(13) 0.0123(14) C23 0.0145(15) 0.0232(16) 0.0186(15) 0.0058(13) 0.0036(12) 0.0113(14) C33 0.0256(18) 0.0225(16) 0.0257(16) 0.0103(14) -0.0065(13) 0.0058(14) C34 0.0173(16) 0.0308(17) 0.0293(17) 0.0148(15) 0.0000(13) 0.0067(14) C35 0.0207(16) 0.0216(15) 0.0213(15) 0.0111(13) 0.0041(12) 0.0078(13) C36 0.0106(14) 0.0196(15) 0.0201(15) 0.0070(12) 0.0035(11) 0.0030(12) C37 0.0196(17) 0.0264(18) 0.0307(18) 0.0097(15) 0.0042(14) 0.0083(14) C41 0.0241(17) 0.0251(16) 0.0217(15) 0.0112(13) 0.0018(13) 0.0061(14) C42 0.0321(19) 0.040(2) 0.0306(18) 0.0200(16) -0.0013(15) 0.0134(17) C43 0.0251(18) 0.0321(18) 0.0273(17) 0.0156(15) 0.0065(14) 0.0082(15) O1_1 0.0344(14) 0.0585(16) 0.0419(14) 0.0289(13) 0.0102(11) 0.0253(13) C2_1 0.029(2) 0.0337(19) 0.052(2) 0.0158(18) 0.0091(17) 0.0105(16) C3_1 0.033(2) 0.059(3) 0.054(3) 0.013(2) -0.0009(19) 0.017(2) C4_1 0.035(2) 0.062(3) 0.049(2) 0.027(2) -0.0047(18) 0.015(2) C1_1 0.037(2) 0.052(2) 0.041(2) 0.0216(19) 0.0112(17) 0.0211(19) 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' K K 0.2009 0.2494 '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' P P 0.1023 0.0942 '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' Si Si 0.0817 0.0704 '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 O2 K1 O3 80.77(6) . . O2 K1 N2 98.38(7) . . O3 K1 N2 74.59(6) . . O2 K1 N1 78.17(6) . . O3 K1 N1 124.81(6) . . N2 K1 N1 158.61(7) . . O2 K1 C44 135.21(8) . . O3 K1 C44 119.88(8) . . N2 K1 C44 57.03(8) . . N1 K1 C44 110.85(8) . . O2 K1 C37 130.23(8) . . O3 K1 C37 58.38(7) . . N2 K1 C37 96.81(8) . . N1 K1 C37 101.46(8) . . C44 K1 C37 92.13(10) . . O2 K1 C36 128.88(7) . . O3 K1 C36 48.15(6) . . N2 K1 C36 73.10(7) . . N1 K1 C36 125.54(7) . . C44 K1 C36 82.84(9) . . C37 K1 C36 24.08(7) . . O2 K1 S2 100.71(5) . . O3 K1 S2 21.42(4) . . N2 K1 S2 63.94(5) . . N1 K1 S2 137.41(5) . . C44 K1 S2 99.68(7) . . C37 K1 S2 46.98(6) . . C36 K1 S2 29.58(5) . . O2 K1 Si2 114.58(5) . . O3 K1 Si2 98.27(4) . . N2 K1 Si2 26.63(5) . . N1 K1 Si2 136.87(5) . . C44 K1 Si2 30.96(6) . . C37 K1 Si2 99.41(6) . . C36 K1 Si2 80.04(5) . . S2 K1 Si2 82.92(2) . . O2 K1 P1 56.68(4) . . O3 K1 P1 106.09(4) . . N2 K1 P1 153.69(5) . . N1 K1 P1 24.30(5) . . C44 K1 P1 133.29(7) . . C37 K1 P1 105.89(6) . . C36 K1 P1 127.58(5) . . S2 K1 P1 124.26(2) . . Si2 K1 P1 151.45(3) . . O2 K1 S1 17.63(4) . . O3 K1 S1 98.10(5) . . N2 K1 S1 106.26(5) . . N1 K1 S1 65.10(5) . . C44 K1 S1 126.45(8) . . C37 K1 S1 141.32(6) . . C36 K1 S1 145.88(5) . . S2 K1 S1 118.31(2) . . Si2 K1 S1 115.15(2) . . P1 K1 S1 47.433(18) . . O2 K1 P2 90.28(5) . . O3 K1 P2 53.80(4) . . N2 K1 P2 21.13(5) . . N1 K1 P2 168.30(5) . . C44 K1 P2 76.10(7) . . C37 K1 P2 87.36(6) . . C36 K1 P2 63.59(5) . . S2 K1 P2 46.228(17) . . Si2 K1 P2 47.108(19) . . P1 K1 P2 145.50(2) . . S1 K1 P2 103.22(2) . . O2 K1 H44C 152.9(8) . . O3 K1 H44C 111.1(8) . . N2 K1 H44C 63.8(8) . . N1 K1 H44C 110.6(8) . . C44 K1 H44C 17.9(8) . . C37 K1 H44C 74.5(8) . . C36 K1 H44C 68.0(8) . . S2 K1 H44C 89.7(8) . . Si2 K1 H44C 41.5(8) . . P1 K1 H44C 134.9(8) . . S1 K1 H44C 143.7(8) . . P2 K1 H44C 79.0(8) . . O2 K1 H44A 123.2(6) . . O3 K1 H44A 137.2(6) . . N2 K1 H44A 67.6(6) . . N1 K1 H44A 96.3(6) . . C44 K1 H44A 18.3(6) . . C37 K1 H44A 106.5(6) . . C36 K1 H44A 100.5(6) . . S2 K1 H44A 117.7(6) . . Si2 K1 H44A 41.3(6) . . P1 K1 H44A 116.7(6) . . S1 K1 H44A 110.9(6) . . P2 K1 H44A 88.4(6) . . H44C K1 H44A 33.0(10) . . S1 O1 K2 133.44(11) . 2_565 N1 Si1 C22 109.00(13) . . N1 Si1 C20 112.17(14) . . C22 Si1 C20 107.72(15) . . N1 Si1 C21 115.39(13) . . C22 Si1 C21 106.08(15) . . C20 Si1 C21 106.06(16) . . N1 Si1 K1 39.65(8) . . C22 Si1 K1 70.90(10) . . C20 Si1 K1 114.77(11) . . C21 Si1 K1 138.04(12) . . P1 N1 Si1 134.44(15) . . P1 N1 K1 107.47(11) . . Si1 N1 K1 118.05(11) . . N1 P1 C1 119.63(13) . . N1 P1 C2 113.38(13) . . C1 P1 C2 102.52(14) . . N1 P1 C8 107.09(13) . . C1 P1 C8 109.06(14) . . C2 P1 C8 104.09(12) . . N1 P1 K1 48.23(9) . . C1 P1 K1 95.02(10) . . C2 P1 K1 160.05(9) . . C8 P1 K1 78.60(9) . . O1 S1 O2 115.22(12) . . O1 S1 C1 112.70(13) . . O2 S1 C1 108.95(13) . . O1 S1 C14 104.15(12) . . O2 S1 C14 103.63(12) . . C1 S1 C14 111.76(14) . . O1 S1 K1 146.45(9) . . O2 S1 K1 32.80(8) . . C1 S1 K1 93.87(11) . . C14 S1 K1 83.09(9) . . O1 S1 K2 84.54(9) . . O2 S1 K2 34.31(8) . . C1 S1 K2 110.62(10) . . C14 S1 K2 128.70(9) . . K1 S1 K2 66.501(19) . . S1 C1 P1 123.05(18) . . S1 C1 H1 116(2) . . P1 C1 H1 120(2) . . O4 K2 O2 169.60(6) 2_665 . O4 K2 O1 85.54(6) 2_665 2_565 O2 K2 O1 104.58(6) . 2_565 O4 K2 O3 93.29(6) 2_665 . O2 K2 O3 79.25(6) . . O1 K2 O3 149.17(6) 2_565 . O4 K2 C31 66.36(7) 2_665 . O2 K2 C31 104.49(7) . . O1 K2 C31 130.14(7) 2_565 . O3 K2 C31 76.00(7) . . O4 K2 C32 63.14(7) 2_665 . O2 K2 C32 110.77(7) . . O1 K2 C32 106.45(7) 2_565 . O3 K2 C32 100.33(7) . . C31 K2 C32 24.37(7) . . O4 K2 C13 121.16(7) 2_665 . O2 K2 C13 66.42(6) . . O1 K2 C13 65.74(7) 2_565 . O3 K2 C13 89.18(7) . . C31 K2 C13 164.10(7) . . C32 K2 C13 169.51(8) . . O4 K2 C30 89.41(7) 2_665 . O2 K2 C30 80.95(6) . . O1 K2 C30 144.91(7) 2_565 . O3 K2 C30 65.72(6) . . C31 K2 C30 24.17(7) . . C32 K2 C30 42.11(7) . . C13 K2 C30 142.29(7) . . O4 K2 C12 97.75(7) 2_665 . O2 K2 C12 89.26(6) . . O1 K2 C12 62.00(7) 2_565 . O3 K2 C12 87.76(7) . . C31 K2 C12 156.07(8) . . C32 K2 C12 159.40(8) . . C13 K2 C12 23.56(7) . . C30 K2 C12 152.94(7) . . O4 K2 S1 169.16(5) 2_665 . O2 K2 S1 17.81(4) . . O1 K2 S1 87.88(5) 2_565 . O3 K2 S1 96.77(4) . . C31 K2 S1 112.24(6) . . C32 K2 S1 110.81(6) . . C13 K2 S1 63.21(5) . . C30 K2 S1 91.04(5) . . C12 K2 S1 86.71(5) . . O4 K2 K1 133.62(5) 2_665 . O2 K2 K1 38.59(4) . . O1 K2 K1 135.04(5) 2_565 . O3 K2 K1 40.66(4) . . C31 K2 K1 91.18(5) . . C32 K2 K1 110.94(5) . . C13 K2 K1 73.58(5) . . C30 K2 K1 69.07(5) . . C12 K2 K1 87.57(5) . . S1 K2 K1 56.147(16) . . S1 O2 K1 129.56(11) . . S1 O2 K2 127.87(11) . . K1 O2 K2 101.41(6) . . N2 Si2 C43 111.78(13) . . N2 Si2 C42 115.13(14) . . C43 Si2 C42 107.47(15) . . N2 Si2 C44 108.63(14) . . C43 Si2 C44 105.37(16) . . C42 Si2 C44 107.96(17) . . N2 Si2 K1 48.60(8) . . C43 Si2 K1 112.74(10) . . C42 Si2 K1 139.80(11) . . C44 Si2 K1 61.45(11) . . P2 N2 Si2 133.31(15) . . P2 N2 K1 118.34(12) . . Si2 N2 K1 104.77(11) . . N2 P2 C23 118.55(14) . . N2 P2 C24 113.08(13) . . C23 P2 C24 105.30(14) . . N2 P2 C30 108.33(13) . . C23 P2 C30 108.26(13) . . C24 P2 C30 101.98(13) . . N2 P2 K1 40.54(9) . . C23 P2 K1 91.23(10) . . C24 P2 K1 153.53(10) . . C30 P2 K1 91.94(9) . . O4 S2 O3 116.17(12) . . O4 S2 C23 111.73(14) . . O3 S2 C23 110.85(13) . . O4 S2 C36 103.61(13) . . O3 S2 C36 102.71(12) . . C23 S2 C36 111.11(14) . . O4 S2 K1 147.04(9) . . O3 S2 K1 42.50(8) . . C23 S2 K1 100.75(11) . . C36 S2 K1 68.08(9) . . C7 C2 C3 118.7(3) . . C7 C2 P1 121.7(2) . . C3 C2 P1 119.3(2) . . C37 C38 C39 120.4(3) . . C37 C38 H38 119.8 . . C39 C38 H38 119.8 . . C8 C13 C12 120.7(3) . . C8 C13 K2 108.98(17) . . C12 C13 K2 81.74(17) . . C8 C13 H13 119.6 . . C12 C13 H13 119.6 . . K2 C13 H13 79.4 . . C18 C17 C16 119.5(3) . . C18 C17 H17 120.3 . . C16 C17 H17 120.3 . . C12 C11 C10 120.2(3) . . C12 C11 H11 119.9 . . C10 C11 H11 119.9 . . C14 C15 C16 120.1(3) . . C14 C15 H15 120.0 . . C16 C15 H15 120.0 . . C19 C14 C15 120.0(3) . . C19 C14 S1 119.9(2) . . C15 C14 S1 120.0(2) . . Si2 C44 K1 87.60(12) . . Si2 C44 H44C 112(2) . . K1 C44 H44C 67(2) . . Si2 C44 H44B 112(2) . . K1 C44 H44B 160(2) . . H44C C44 H44B 109(3) . . Si2 C44 H44A 108.7(17) . . K1 C44 H44A 61.1(16) . . H44C C44 H44A 110(3) . . H44B C44 H44A 105(3) . . C17 C16 C15 120.0(3) . . C17 C16 H16 120.0 . . C15 C16 H16 120.0 . . C39 C40 C41 120.2(3) . . C39 C40 H40 119.9 . . C41 C40 H40 119.9 . . C38 C39 C40 119.8(3) . . C38 C39 H39 120.1 . . C40 C39 H39 120.1 . . C4 C3 C2 120.4(3) . . C4 C3 H3 119.8 . . C2 C3 H3 119.8 . . S2 O3 K1 116.09(10) . . S2 O3 K2 139.89(11) . . K1 O3 K2 98.56(6) . . C3 C4 C5 120.3(3) . . C3 C4 H4 119.9 . . C5 C4 H4 119.9 . . S2 O4 K2 147.20(12) . 2_665 C6 C5 C4 119.8(3) . . C6 C5 H5 120.1 . . C4 C5 H5 120.1 . . C5 C6 C7 120.2(3) . . C5 C6 H6 119.9 . . C7 C6 H6 119.9 . . C6 C7 C2 120.6(3) . . C6 C7 H7 119.7 . . C2 C7 H7 119.7 . . C9 C8 C13 118.7(3) . . C9 C8 P1 119.1(2) . . C13 C8 P1 122.1(2) . . C10 C9 C8 120.7(3) . . C10 C9 H9 119.7 . . C8 C9 H9 119.7 . . C11 C10 C9 120.1(3) . . C11 C10 H10 119.9 . . C9 C10 H10 119.9 . . C11 C12 C13 119.5(3) . . C11 C12 K2 113.77(19) . . C13 C12 K2 74.70(16) . . C11 C12 H12 120.2 . . C13 C12 H12 120.2 . . K2 C12 H12 82.1 . . Si1 C21 H21A 109.5 . . Si1 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . Si1 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . Si1 C20 H20A 109.5 . . Si1 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . Si1 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C14 C19 C18 119.7(3) . . C14 C19 H19 120.2 . . C18 C19 H19 120.2 . . C17 C18 C19 120.7(3) . . C17 C18 H18 119.6 . . C19 C18 H18 119.6 . . Si1 C22 H22A 109.5 . . Si1 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . Si1 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C33 C32 C31 120.1(3) . . C33 C32 K2 88.36(18) . . C31 C32 K2 73.82(16) . . C33 C32 H32 120.7(18) . . C31 C32 H32 119.1(18) . . K2 C32 H32 108.3(17) . . C32 C31 C30 120.3(3) . . C32 C31 K2 81.81(17) . . C30 C31 K2 84.02(17) . . C32 C31 H31 123.9(17) . . C30 C31 H31 115.7(17) . . K2 C31 H31 103.6(16) . . C35 C30 C31 119.1(3) . . C35 C30 P2 120.3(2) . . C31 C30 P2 120.5(2) . . C35 C30 K2 86.91(16) . . C31 C30 K2 71.81(16) . . P2 C30 K2 113.98(11) . . C28 C29 C24 121.4(3) . . C28 C29 H29 119.3 . . C24 C29 H29 119.3 . . C27 C28 C29 119.6(3) . . C27 C28 H28 120.2 . . C29 C28 H28 120.2 . . C26 C27 C28 120.1(3) . . C26 C27 H27 119.9 . . C28 C27 H27 119.9 . . C27 C26 C25 120.5(3) . . C27 C26 H26 119.7 . . C25 C26 H26 119.7 . . C24 C25 C26 120.5(3) . . C24 C25 H25 119.8 . . C26 C25 H25 119.8 . . C25 C24 C29 117.9(3) . . C25 C24 P2 124.3(2) . . C29 C24 P2 117.4(2) . . S2 C23 P2 120.09(18) . . S2 C23 H23 121(3) . . P2 C23 H23 119(3) . . C34 C33 C32 119.8(3) . . C34 C33 H33 120.1 . . C32 C33 H33 120.1 . . C33 C34 C35 120.3(3) . . C33 C34 H34 119.9 . . C35 C34 H34 119.9 . . C34 C35 C30 120.3(3) . . C34 C35 H35 119.8 . . C30 C35 H35 119.8 . . C41 C36 C37 119.8(3) . . C41 C36 S2 120.8(2) . . C37 C36 S2 119.4(2) . . C41 C36 K1 115.22(19) . . C37 C36 K1 73.80(17) . . S2 C36 K1 82.34(10) . . C38 C37 C36 120.1(3) . . C38 C37 K1 109.5(2) . . C36 C37 K1 82.12(17) . . C38 C37 H37 123(2) . . C36 C37 H37 117(2) . . K1 C37 H37 81(2) . . C36 C41 C40 119.7(3) . . C36 C41 H41 120.1 . . C40 C41 H41 120.1 . . Si2 C42 H42A 109.5 . . Si2 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . Si2 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . Si2 C43 H43A 109.5 . . Si2 C43 H43B 109.5 . . H43A C43 H43B 109.5 . . Si2 C43 H43C 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C4_1 O1_1 C1_1 108.6(3) . . C3_1 C2_1 C1_1 102.5(3) . . C3_1 C2_1 H2A_1 111.3 . . C1_1 C2_1 H2A_1 111.3 . . C3_1 C2_1 H2B_1 111.3 . . C1_1 C2_1 H2B_1 111.3 . . H2A_1 C2_1 H2B_1 109.2 . . C2_1 C3_1 C4_1 103.6(3) . . C2_1 C3_1 H3A_1 111.0 . . C4_1 C3_1 H3A_1 111.0 . . C2_1 C3_1 H3B_1 111.0 . . C4_1 C3_1 H3B_1 111.0 . . H3A_1 C3_1 H3B_1 109.0 . . O1_1 C4_1 C3_1 106.1(3) . . O1_1 C4_1 H4A_1 110.5 . . C3_1 C4_1 H4A_1 110.5 . . O1_1 C4_1 H4B_1 110.5 . . C3_1 C4_1 H4B_1 110.5 . . H4A_1 C4_1 H4B_1 108.7 . . O1_1 C1_1 C2_1 106.6(3) . . O1_1 C1_1 H1A_1 110.4 . . C2_1 C1_1 H1A_1 110.4 . . O1_1 C1_1 H1B_1 110.4 . . C2_1 C1_1 H1B_1 110.4 . . H1A_1 C1_1 H1B_1 108.6 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K1 O2 2.611(2) . K1 O3 2.704(2) . K1 N2 2.817(2) . K1 N1 2.843(2) . K1 C44 3.192(4) . K1 C37 3.262(3) . K1 C36 3.365(3) . K1 S2 3.5948(9) . K1 Si2 3.6310(10) . K1 P1 3.6367(9) . K1 S1 3.7161(10) . K1 P2 3.8144(10) . K1 H44C 2.94(4) . K1 H44A 2.84(3) . O1 S1 1.446(2) . O1 K2 2.703(2) 2_565 Si1 N1 1.691(2) . Si1 C22 1.864(3) . Si1 C20 1.866(3) . Si1 C21 1.867(3) . N1 P1 1.569(2) . P1 C1 1.728(3) . P1 C2 1.820(3) . P1 C8 1.823(3) . S1 O2 1.4602(19) . S1 C1 1.637(3) . S1 C14 1.787(3) . S1 K2 3.7678(9) . C1 H1 0.84(3) . K2 O4 2.593(2) 2_665 K2 O2 2.6907(19) . K2 O1 2.703(2) 2_565 K2 O3 2.711(2) . K2 C31 3.223(3) . K2 C32 3.321(3) . K2 C13 3.354(3) . K2 C30 3.374(3) . K2 C12 3.441(3) . Si2 N2 1.683(2) . Si2 C43 1.855(3) . Si2 C42 1.867(3) . Si2 C44 1.869(4) . N2 P2 1.562(2) . P2 C23 1.726(3) . P2 C24 1.813(3) . P2 C30 1.820(3) . S2 O4 1.444(2) . S2 O3 1.462(2) . S2 C23 1.639(3) . S2 C36 1.790(3) . C2 C7 1.385(4) . C2 C3 1.392(4) . C38 C37 1.364(5) . C38 C39 1.375(5) . C38 H38 0.9500 . C13 C8 1.384(4) . C13 C12 1.390(4) . C13 H13 0.9500 . C17 C18 1.365(5) . C17 C16 1.380(5) . C17 H17 0.9500 . C11 C12 1.375(4) . C11 C10 1.376(5) . C11 H11 0.9500 . C15 C14 1.374(4) . C15 C16 1.382(5) . C15 H15 0.9500 . C14 C19 1.370(4) . C44 H44C 0.99(4) . C44 H44B 0.98(4) . C44 H44A 1.02(3) . C16 H16 0.9500 . C40 C39 1.378(5) . C40 C41 1.379(4) . C40 H40 0.9500 . C39 H39 0.9500 . C3 C4 1.374(4) . C3 H3 0.9500 . C4 C5 1.381(4) . C4 H4 0.9500 . O4 K2 2.593(2) 2_665 C5 C6 1.372(4) . C5 H5 0.9500 . C6 C7 1.380(4) . C6 H6 0.9500 . C7 H7 0.9500 . C8 C9 1.382(4) . C9 C10 1.380(4) . C9 H9 0.9500 . C10 H10 0.9500 . C12 H12 0.9500 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C19 C18 1.385(4) . C19 H19 0.9500 . C18 H18 0.9500 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C32 C33 1.381(4) . C32 C31 1.385(4) . C32 H32 1.01(3) . C31 C30 1.389(4) . C31 H31 0.95(3) . C30 C35 1.389(4) . C29 C28 1.378(4) . C29 C24 1.386(4) . C29 H29 0.9500 . C28 C27 1.373(5) . C28 H28 0.9500 . C27 C26 1.359(5) . C27 H27 0.9500 . C26 C25 1.385(5) . C26 H26 0.9500 . C25 C24 1.384(4) . C25 H25 0.9500 . C23 H23 0.79(4) . C33 C34 1.378(4) . C33 H33 0.9500 . C34 C35 1.384(4) . C34 H34 0.9500 . C35 H35 0.9500 . C36 C41 1.377(4) . C36 C37 1.386(4) . C37 H37 0.89(3) . C41 H41 0.9500 . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . O1_1 C4_1 1.428(4) . O1_1 C1_1 1.435(4) . C2_1 C3_1 1.478(5) . C2_1 C1_1 1.522(5) . C2_1 H2A_1 0.9900 . C2_1 H2B_1 0.9900 . C3_1 C4_1 1.487(5) . C3_1 H3A_1 0.9900 . C3_1 H3B_1 0.9900 . C4_1 H4A_1 0.9900 . C4_1 H4B_1 0.9900 . C1_1 H1A_1 0.9900 . C1_1 H1B_1 0.9900 . 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 C22 Si1 N1 P1 -160.8(2) . . . . C20 Si1 N1 P1 80.0(2) . . . . C21 Si1 N1 P1 -41.6(3) . . . . K1 Si1 N1 P1 -177.4(3) . . . . C22 Si1 N1 K1 16.64(17) . . . . C20 Si1 N1 K1 -102.56(15) . . . . C21 Si1 N1 K1 135.84(14) . . . . Si1 N1 P1 C1 -114.3(2) . . . . K1 N1 P1 C1 68.09(16) . . . . Si1 N1 P1 C2 6.9(3) . . . . K1 N1 P1 C2 -170.74(11) . . . . Si1 N1 P1 C8 121.1(2) . . . . K1 N1 P1 C8 -56.51(14) . . . . Si1 N1 P1 K1 177.6(3) . . . . K2 O1 S1 O2 -113.95(16) 2_565 . . . K2 O1 S1 C1 11.9(2) 2_565 . . . K2 O1 S1 C14 133.26(16) 2_565 . . . K2 O1 S1 K1 -127.80(12) 2_565 . . . K2 O1 S1 K2 -98.15(14) 2_565 . . . O1 S1 C1 P1 -150.77(17) . . . . O2 S1 C1 P1 -21.6(2) . . . . C14 S1 C1 P1 92.3(2) . . . . K1 S1 C1 P1 8.25(18) . . . . K2 S1 C1 P1 -58.1(2) . . . . N1 P1 C1 S1 -52.4(2) . . . . C2 P1 C1 S1 -178.88(18) . . . . C8 P1 C1 S1 71.2(2) . . . . K1 P1 C1 S1 -8.45(19) . . . . O1 S1 O2 K1 -165.87(12) . . . . C1 S1 O2 K1 66.34(17) . . . . C14 S1 O2 K1 -52.78(16) . . . . K2 S1 O2 K1 165.4(2) . . . . O1 S1 O2 K2 28.73(17) . . . . C1 S1 O2 K2 -99.06(16) . . . . C14 S1 O2 K2 141.82(14) . . . . K1 S1 O2 K2 -165.4(2) . . . . C43 Si2 N2 P2 -100.9(2) . . . . C42 Si2 N2 P2 22.1(3) . . . . C44 Si2 N2 P2 143.2(2) . . . . K1 Si2 N2 P2 157.4(3) . . . . C43 Si2 N2 K1 101.69(13) . . . . C42 Si2 N2 K1 -135.32(13) . . . . C44 Si2 N2 K1 -14.16(17) . . . . Si2 N2 P2 C23 -101.8(2) . . . . K1 N2 P2 C23 53.21(18) . . . . Si2 N2 P2 C24 22.1(3) . . . . K1 N2 P2 C24 177.16(12) . . . . Si2 N2 P2 C30 134.4(2) . . . . K1 N2 P2 C30 -70.57(15) . . . . Si2 N2 P2 K1 -155.0(3) . . . . N1 P1 C2 C7 93.0(3) . . . . C1 P1 C2 C7 -136.7(2) . . . . C8 P1 C2 C7 -23.1(3) . . . . K1 P1 C2 C7 72.4(4) . . . . N1 P1 C2 C3 -79.9(3) . . . . C1 P1 C2 C3 50.5(3) . . . . C8 P1 C2 C3 164.1(2) . . . . K1 P1 C2 C3 -100.5(3) . . . . C16 C15 C14 C19 0.3(5) . . . . C16 C15 C14 S1 177.9(3) . . . . O1 S1 C14 C19 -147.6(3) . . . . O2 S1 C14 C19 91.5(3) . . . . C1 S1 C14 C19 -25.7(3) . . . . K1 S1 C14 C19 65.8(2) . . . . K2 S1 C14 C19 118.0(2) . . . . O1 S1 C14 C15 34.8(3) . . . . O2 S1 C14 C15 -86.1(3) . . . . C1 S1 C14 C15 156.7(3) . . . . K1 S1 C14 C15 -111.9(3) . . . . K2 S1 C14 C15 -59.6(3) . . . . N2 Si2 C44 K1 12.06(14) . . . . C43 Si2 C44 K1 -107.86(12) . . . . C42 Si2 C44 K1 137.53(12) . . . . C18 C17 C16 C15 -2.7(6) . . . . C14 C15 C16 C17 1.7(6) . . . . C37 C38 C39 C40 -0.2(5) . . . . C41 C40 C39 C38 -0.6(5) . . . . C7 C2 C3 C4 -0.3(4) . . . . P1 C2 C3 C4 172.8(2) . . . . O4 S2 O3 K1 -147.95(11) . . . . C23 S2 O3 K1 83.10(15) . . . . C36 S2 O3 K1 -35.65(14) . . . . O4 S2 O3 K2 65.1(2) . . . . C23 S2 O3 K2 -63.8(2) . . . . C36 S2 O3 K2 177.40(16) . . . . K1 S2 O3 K2 -146.9(2) . . . . C2 C3 C4 C5 -0.2(5) . . . . O3 S2 O4 K2 -111.3(2) . . . 2_665 C23 S2 O4 K2 17.2(3) . . . 2_665 C36 S2 O4 K2 136.9(2) . . . 2_665 K1 S2 O4 K2 -152.52(12) . . . 2_665 C3 C4 C5 C6 0.6(5) . . . . C4 C5 C6 C7 -0.6(5) . . . . C5 C6 C7 C2 0.1(5) . . . . C3 C2 C7 C6 0.3(4) . . . . P1 C2 C7 C6 -172.5(2) . . . . C12 C13 C8 C9 0.6(4) . . . . K2 C13 C8 C9 92.2(3) . . . . C12 C13 C8 P1 177.9(2) . . . . K2 C13 C8 P1 -90.5(2) . . . . N1 P1 C8 C9 -33.4(3) . . . . C1 P1 C8 C9 -164.2(2) . . . . C2 P1 C8 C9 86.9(2) . . . . K1 P1 C8 C9 -72.8(2) . . . . N1 P1 C8 C13 149.2(2) . . . . C1 P1 C8 C13 18.4(3) . . . . C2 P1 C8 C13 -90.4(2) . . . . K1 P1 C8 C13 109.8(2) . . . . C13 C8 C9 C10 0.9(4) . . . . P1 C8 C9 C10 -176.5(2) . . . . C12 C11 C10 C9 0.0(5) . . . . C8 C9 C10 C11 -1.2(5) . . . . C10 C11 C12 C13 1.5(4) . . . . C10 C11 C12 K2 -83.9(3) . . . . C8 C13 C12 C11 -1.8(4) . . . . K2 C13 C12 C11 -109.0(3) . . . . C8 C13 C12 K2 107.2(3) . . . . C15 C14 C19 C18 -1.2(5) . . . . S1 C14 C19 C18 -178.8(3) . . . . C16 C17 C18 C19 1.8(6) . . . . C14 C19 C18 C17 0.1(6) . . . . C33 C32 C31 C30 -0.2(4) . . . . K2 C32 C31 C30 78.1(2) . . . . C33 C32 C31 K2 -78.3(3) . . . . C32 C31 C30 C35 -1.2(4) . . . . K2 C31 C30 C35 75.7(2) . . . . C32 C31 C30 P2 175.5(2) . . . . K2 C31 C30 P2 -107.63(18) . . . . C32 C31 C30 K2 -76.9(2) . . . . N2 P2 C30 C35 -24.0(3) . . . . C23 P2 C30 C35 -153.8(2) . . . . C24 P2 C30 C35 95.5(2) . . . . K1 P2 C30 C35 -61.9(2) . . . . N2 P2 C30 C31 159.3(2) . . . . C23 P2 C30 C31 29.5(3) . . . . C24 P2 C30 C31 -81.2(2) . . . . K1 P2 C30 C31 121.5(2) . . . . N2 P2 C30 K2 77.01(14) . . . . C23 P2 C30 K2 -52.75(16) . . . . C24 P2 C30 K2 -163.48(12) . . . . K1 P2 C30 K2 39.18(10) . . . . C24 C29 C28 C27 0.8(5) . . . . C29 C28 C27 C26 -0.3(6) . . . . C28 C27 C26 C25 -0.8(6) . . . . C27 C26 C25 C24 1.4(6) . . . . C26 C25 C24 C29 -0.9(5) . . . . C26 C25 C24 P2 171.5(3) . . . . C28 C29 C24 C25 -0.2(5) . . . . C28 C29 C24 P2 -173.1(2) . . . . N2 P2 C24 C25 -110.4(3) . . . . C23 P2 C24 C25 20.5(3) . . . . C30 P2 C24 C25 133.5(3) . . . . K1 P2 C24 C25 -106.3(3) . . . . N2 P2 C24 C29 62.0(3) . . . . C23 P2 C24 C29 -167.0(2) . . . . C30 P2 C24 C29 -54.1(3) . . . . K1 P2 C24 C29 66.2(3) . . . . O4 S2 C23 P2 -160.38(16) . . . . O3 S2 C23 P2 -29.1(2) . . . . C36 S2 C23 P2 84.5(2) . . . . K1 S2 C23 P2 13.96(19) . . . . N2 P2 C23 S2 -44.3(2) . . . . C24 P2 C23 S2 -171.99(17) . . . . C30 P2 C23 S2 79.5(2) . . . . K1 P2 C23 S2 -12.91(18) . . . . C31 C32 C33 C34 1.3(4) . . . . K2 C32 C33 C34 -68.9(3) . . . . C32 C33 C34 C35 -1.0(5) . . . . C33 C34 C35 C30 -0.4(4) . . . . C31 C30 C35 C34 1.5(4) . . . . P2 C30 C35 C34 -175.2(2) . . . . K2 C30 C35 C34 68.7(3) . . . . O4 S2 C36 C41 -98.7(2) . . . . O3 S2 C36 C41 140.0(2) . . . . C23 S2 C36 C41 21.4(3) . . . . K1 S2 C36 C41 114.9(2) . . . . O4 S2 C36 C37 79.9(3) . . . . O3 S2 C36 C37 -41.4(3) . . . . C23 S2 C36 C37 -159.9(2) . . . . K1 S2 C36 C37 -66.5(2) . . . . O4 S2 C36 K1 146.43(9) . . . . O3 S2 C36 K1 25.11(10) . . . . C23 S2 C36 K1 -93.46(13) . . . . C39 C38 C37 C36 1.6(5) . . . . C39 C38 C37 K1 93.7(3) . . . . C41 C36 C37 C38 -2.2(5) . . . . S2 C36 C37 C38 179.2(2) . . . . K1 C36 C37 C38 108.0(3) . . . . C41 C36 C37 K1 -110.2(3) . . . . S2 C36 C37 K1 71.15(19) . . . . C37 C36 C41 C40 1.4(5) . . . . S2 C36 C41 C40 -180.0(2) . . . . K1 C36 C41 C40 -83.7(3) . . . . C39 C40 C41 C36 0.0(5) . . . . C1_1 C2_1 C3_1 C4_1 34.5(4) . . . . C1_1 O1_1 C4_1 C3_1 18.1(4) . . . . C2_1 C3_1 C4_1 O1_1 -33.4(4) . . . . C4_1 O1_1 C1_1 C2_1 4.0(4) . . . . C3_1 C2_1 C1_1 O1_1 -24.3(4) . . . .