#------------------------------------------------------------------------------ #$Date: 2014-12-19 10:20:53 +0200 (Fri, 19 Dec 2014) $ #$Revision: 128844 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116057.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_7116057 loop_ _publ_author_name 'P. Steiniger' 'G. Bendt' 'D. Blaser' 'C. Wolper' 'S. Schulz' _publ_section_title ; Germane vs. digermane formation ; _journal_name_full Chem.Commun. _journal_page_first 15461 _journal_paper_doi 10.1039/C4cc07921C _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C24 H58 Ge2 N4 Se2 Si2' _chemical_formula_sum 'C24 H58 Ge2 N4 Se2 Si2' _chemical_formula_weight 762.02 _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/5 _cell_angle_alpha 113.426(3) _cell_angle_beta 90.896(3) _cell_angle_gamma 99.856(3) _cell_formula_units_Z 4 _cell_length_a 11.9600(7) _cell_length_b 18.0926(11) _cell_length_c 18.1839(11) _cell_measurement_reflns_used 23513 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 28.114 _cell_measurement_theta_min 2.297 _cell_volume 3541.9(4) _computing_cell_refinement 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_data_collection 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_data_reduction 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_molecular_graphics 'BRUKER AXS Inc. 2008 Vers. 2008/4' _computing_publication_material 'SHELXL-2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/5 (Sheldrick, 2014)' _computing_structure_solution 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _diffrn_ambient_temperature 100(1) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type ; Bruker D8 KAPPA series II with APEX II area detector system ; _diffrn_measurement_method ; Data collection strategy APEX 2/COSMO ; _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_laue_measured_fraction_full 0.997 _diffrn_reflns_laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 101681 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.178 _diffrn_reflns_theta_min 1.349 _diffrn_source 'sealed X-RAY tube' _exptl_absorpt_coefficient_mu 3.839 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 3.0-2009 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.429 _exptl_crystal_description block _exptl_crystal_F_000 1560 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.110 _refine_diff_density_max 2.720 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 649 _refine_ls_number_reflns 17182 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0382 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+7.4020P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.0923 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12899 _reflns_number_total 17182 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc07921c2.cif _[local]_cod_data_source_block pst_074m _cod_database_code 7116057 _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 0.413 _shelx_estimated_absorpt_t_max 0.677 _shelxl_version_number 2014/5 _shelx_res_file ; TITL pst_074m in P-1 CELL 0.71073 11.9600 18.0926 18.1839 113.426 90.896 99.856 ZERR 4.00 0.0007 0.0011 0.0011 0.003 0.003 0.003 LATT 1 SFAC C H N SI GE SE UNIT 96 232 16 8 8 8 TEMP -173 SIZE 0.28 0.13 0.11 L.S. 12 ACTA FMAP 2 PLAN 11 WGHT 0.037800 7.402000 FVAR 0.06322 SE1 6 0.206487 0.604494 0.164010 11.00000 0.01529 0.01538 = 0.01582 0.00168 0.00106 0.00551 GE1 5 0.173529 0.720533 0.275956 11.00000 0.01067 0.01237 = 0.01203 0.00378 0.00104 0.00301 SI1 4 0.335140 0.817907 0.390673 11.00000 0.01341 0.01789 = 0.02002 0.00174 -0.00325 0.00304 N1 3 0.279971 0.815825 0.300954 11.00000 0.01547 0.01068 = 0.01966 0.00392 0.00121 -0.00154 N2 3 0.236697 0.728887 0.373179 11.00000 0.01889 0.01855 = 0.01409 0.00584 -0.00346 0.00083 C1 1 0.489797 0.811398 0.394166 11.00000 0.01752 0.02615 = 0.03891 0.00720 -0.00535 0.00406 AFIX 137 H1A 2 0.502999 0.764712 0.346350 11.00000 -1.50000 H1B 2 0.511200 0.803895 0.442626 11.00000 -1.50000 H1C 2 0.536019 0.862185 0.395349 11.00000 -1.50000 AFIX 0 C2 1 0.322365 0.908877 0.484218 11.00000 0.02732 0.02558 = 0.02874 -0.00211 -0.00621 0.00258 AFIX 137 H2A 2 0.371338 0.958064 0.483931 11.00000 -1.50000 H2B 2 0.346053 0.900024 0.531436 11.00000 -1.50000 H2C 2 0.243007 0.916237 0.486332 11.00000 -1.50000 AFIX 0 C3 1 0.318030 0.859231 0.249994 11.00000 0.01589 0.02035 = 0.03235 0.01498 0.00472 0.00221 C4 1 0.365164 0.948833 0.303446 11.00000 0.03134 0.02070 = 0.04744 0.01431 0.00392 -0.00245 AFIX 137 H4A 2 0.306892 0.972464 0.337705 11.00000 -1.50000 H4B 2 0.386592 0.979019 0.269818 11.00000 -1.50000 H4C 2 0.432415 0.952820 0.337298 11.00000 -1.50000 AFIX 0 C5 1 0.215819 0.854679 0.195252 11.00000 0.01940 0.03675 = 0.03937 0.02644 0.00584 0.00640 AFIX 137 H5A 2 0.184412 0.797134 0.160439 11.00000 -1.50000 H5B 2 0.240597 0.884680 0.161971 11.00000 -1.50000 H5C 2 0.157167 0.879314 0.228381 11.00000 -1.50000 AFIX 0 C6 1 0.408815 0.820562 0.197133 11.00000 0.02460 0.03692 = 0.03987 0.02273 0.01650 0.01143 AFIX 137 H6A 2 0.475136 0.823906 0.231455 11.00000 -1.50000 H6B 2 0.432071 0.850182 0.163271 11.00000 -1.50000 H6C 2 0.377272 0.762880 0.162883 11.00000 -1.50000 AFIX 0 C7 1 0.204957 0.682689 0.423246 11.00000 0.01997 0.03244 = 0.02181 0.01591 0.00197 0.00664 C8 1 0.120666 0.722201 0.482593 11.00000 0.02621 0.04129 = 0.02076 0.01654 0.00390 0.00849 AFIX 137 H8A 2 0.155261 0.779349 0.516681 11.00000 -1.50000 H8B 2 0.102051 0.691821 0.516393 11.00000 -1.50000 H8C 2 0.050905 0.720641 0.452571 11.00000 -1.50000 AFIX 0 C9 1 0.153354 0.593618 0.370438 11.00000 0.03264 0.02828 = 0.03075 0.01972 0.00732 0.00885 AFIX 137 H9A 2 0.084460 0.591140 0.338979 11.00000 -1.50000 H9B 2 0.133654 0.563570 0.404410 11.00000 -1.50000 H9C 2 0.208678 0.568718 0.333878 11.00000 -1.50000 AFIX 0 C10 1 0.314316 0.685957 0.471402 11.00000 0.03096 0.05067 = 0.02844 0.02463 -0.00333 0.00970 AFIX 137 H10A 2 0.368554 0.660588 0.434062 11.00000 -1.50000 H10B 2 0.295372 0.656080 0.505612 11.00000 -1.50000 H10C 2 0.348527 0.743282 0.505138 11.00000 -1.50000 AFIX 0 C11 1 0.361207 0.602626 0.200719 11.00000 0.02046 0.03002 = 0.02252 0.01012 0.00299 0.01198 AFIX 23 H11A 2 0.394652 0.656717 0.243946 11.00000 -1.20000 H11B 2 0.357316 0.560720 0.223239 11.00000 -1.20000 AFIX 0 C12 1 0.436311 0.583331 0.132418 11.00000 0.01862 0.05217 = 0.03565 0.01859 0.00853 0.01749 AFIX 137 H12A 2 0.399215 0.532764 0.087263 11.00000 -1.50000 H12B 2 0.509652 0.575978 0.150461 11.00000 -1.50000 H12C 2 0.448930 0.628697 0.115093 11.00000 -1.50000 AFIX 0 GE21 5 -0.031201 0.723906 0.253146 11.00000 0.01135 0.01394 = 0.01201 0.00375 0.00109 0.00207 SE21 6 -0.131268 0.644759 0.316737 11.00000 0.01509 0.03376 = 0.02643 0.02040 0.00062 0.00056 SI21 4 -0.136459 0.796895 0.180325 11.00000 0.01485 0.01880 = 0.02097 0.00908 0.00093 0.00431 N21 3 -0.101474 0.700546 0.152883 11.00000 0.01508 0.01765 = 0.01148 0.00324 -0.00212 0.00581 N22 3 -0.071461 0.824894 0.276290 11.00000 0.01559 0.01348 = 0.01958 0.00048 0.00091 0.00644 C21 1 -0.292500 0.798985 0.175998 11.00000 0.01818 0.02839 = 0.03465 0.01045 -0.00252 0.00811 AFIX 137 H21A 2 -0.331972 0.764660 0.201551 11.00000 -1.50000 H21B 2 -0.323543 0.777836 0.119696 11.00000 -1.50000 H21C 2 -0.303578 0.855554 0.204485 11.00000 -1.50000 AFIX 0 C22 1 -0.073272 0.856748 0.122072 11.00000 0.02767 0.03714 = 0.04416 0.03012 0.00069 0.00786 AFIX 137 H22A 2 -0.087981 0.912730 0.146828 11.00000 -1.50000 H22B 2 -0.107986 0.830059 0.066383 11.00000 -1.50000 H22C 2 0.009143 0.858707 0.122589 11.00000 -1.50000 AFIX 0 C23 1 -0.107040 0.631670 0.074392 11.00000 0.01687 0.02469 = 0.01390 -0.00048 -0.00172 0.00717 C24 1 -0.215985 0.624098 0.023865 11.00000 0.02920 0.04110 = 0.02052 0.00000 -0.00689 0.01196 AFIX 137 H24A 2 -0.282539 0.616353 0.052652 11.00000 -1.50000 H24B 2 -0.222054 0.576877 -0.027992 11.00000 -1.50000 H24C 2 -0.212831 0.674234 0.014716 11.00000 -1.50000 AFIX 0 C25 1 -0.111906 0.551864 0.085946 11.00000 0.02369 0.01917 = 0.02351 -0.00119 0.00201 0.00245 AFIX 137 H25A 2 -0.042826 0.555981 0.118162 11.00000 -1.50000 H25B 2 -0.117063 0.505848 0.033293 11.00000 -1.50000 H25C 2 -0.178942 0.542693 0.113779 11.00000 -1.50000 AFIX 0 C26 1 -0.003007 0.645218 0.030050 11.00000 0.02976 0.03528 = 0.01784 0.00801 0.00442 0.01400 AFIX 137 H26A 2 -0.000898 0.695417 0.021175 11.00000 -1.50000 H26B 2 -0.008037 0.598289 -0.021924 11.00000 -1.50000 H26C 2 0.066528 0.650622 0.062505 11.00000 -1.50000 AFIX 0 C27 1 -0.070237 0.893126 0.353939 11.00000 0.01843 0.01766 = 0.02408 -0.00538 0.00079 0.00557 C28 1 -0.177221 0.878932 0.395502 11.00000 0.02612 0.03505 = 0.03018 -0.00609 0.01004 0.00832 AFIX 137 H28A 2 -0.244963 0.874386 0.361797 11.00000 -1.50000 H28B 2 -0.173818 0.925210 0.447770 11.00000 -1.50000 H28C 2 -0.181326 0.828119 0.403531 11.00000 -1.50000 AFIX 0 C29 1 -0.064868 0.972132 0.340208 11.00000 0.03788 0.01948 = 0.04332 0.00095 -0.00256 0.00996 AFIX 137 H29A 2 0.001428 0.979761 0.311157 11.00000 -1.50000 H29B 2 -0.058102 1.019171 0.392266 11.00000 -1.50000 H29C 2 -0.134506 0.967836 0.308446 11.00000 -1.50000 AFIX 0 C30 1 0.035775 0.902043 0.406783 11.00000 0.02583 0.02755 = 0.02267 -0.00675 -0.00388 0.01113 AFIX 137 H30A 2 0.032459 0.852071 0.416253 11.00000 -1.50000 H30B 2 0.039110 0.949198 0.458377 11.00000 -1.50000 H30C 2 0.103884 0.910592 0.379679 11.00000 -1.50000 AFIX 0 C31 1 -0.285323 0.645175 0.277535 11.00000 0.01567 0.02694 = 0.02252 0.01508 0.00181 0.00151 AFIX 23 H31A 2 -0.291246 0.701408 0.284359 11.00000 -1.20000 H31B 2 -0.300726 0.608674 0.219562 11.00000 -1.20000 AFIX 0 C32 1 -0.371842 0.615551 0.324907 11.00000 0.01625 0.03790 = 0.02794 0.01783 0.00546 0.00561 AFIX 137 H32A 2 -0.360747 0.562105 0.322121 11.00000 -1.50000 H32B 2 -0.449014 0.610180 0.301965 11.00000 -1.50000 H32C 2 -0.361609 0.655248 0.381214 11.00000 -1.50000 AFIX 0 SE41 6 0.651263 0.395951 0.341524 11.00000 0.01439 0.01729 = 0.01323 0.00230 0.00233 -0.00107 GE41 5 0.553732 0.285012 0.224789 11.00000 0.01023 0.01295 = 0.01185 0.00350 0.00283 0.00101 SI41 4 0.660081 0.190891 0.107866 11.00000 0.01335 0.01493 = 0.01717 0.00350 0.00587 0.00399 N41 3 0.604982 0.186890 0.194516 11.00000 0.01823 0.01220 = 0.01470 0.00573 0.00180 0.00385 N42 3 0.614361 0.282621 0.130505 11.00000 0.01829 0.01647 = 0.01296 0.00514 0.00700 0.00424 C41 1 0.595512 0.106513 0.010118 11.00000 0.02984 0.01806 = 0.01927 0.00332 0.00860 0.00709 AFIX 137 H41A 2 0.513072 0.103952 0.005306 11.00000 -1.50000 H41B 2 0.610335 0.054133 0.008056 11.00000 -1.50000 H41C 2 0.629219 0.117140 -0.034344 11.00000 -1.50000 AFIX 0 C42 1 0.817071 0.194610 0.106934 11.00000 0.01930 0.02809 = 0.03301 0.01100 0.00880 0.00672 AFIX 137 H42A 2 0.843974 0.206037 0.061193 11.00000 -1.50000 H42B 2 0.833495 0.141668 0.101963 11.00000 -1.50000 H42C 2 0.856111 0.238078 0.157157 11.00000 -1.50000 AFIX 0 C43 1 0.617714 0.138261 0.241196 11.00000 0.02097 0.01428 = 0.02147 0.00845 0.00122 0.00278 C44 1 0.603888 0.048040 0.183472 11.00000 0.04212 0.01822 = 0.02927 0.00956 0.00483 0.01102 AFIX 137 H44A 2 0.530368 0.030382 0.151066 11.00000 -1.50000 H44B 2 0.606816 0.014591 0.214379 11.00000 -1.50000 H44C 2 0.665611 0.041266 0.147937 11.00000 -1.50000 AFIX 0 C45 1 0.524605 0.147396 0.299147 11.00000 0.02456 0.01997 = 0.02772 0.01291 0.00233 0.00125 AFIX 137 H45A 2 0.532320 0.205270 0.335929 11.00000 -1.50000 H45B 2 0.532228 0.114678 0.330206 11.00000 -1.50000 H45C 2 0.449605 0.128093 0.268439 11.00000 -1.50000 AFIX 0 C46 1 0.734849 0.167830 0.290279 11.00000 0.01936 0.04258 = 0.03601 0.02355 -0.00189 0.00594 AFIX 137 H46A 2 0.795154 0.160900 0.253595 11.00000 -1.50000 H46B 2 0.740581 0.135468 0.321971 11.00000 -1.50000 H46C 2 0.743376 0.225943 0.326517 11.00000 -1.50000 AFIX 0 C47 1 0.608348 0.332506 0.084226 11.00000 0.02036 0.01845 = 0.01799 0.00837 0.00526 0.00319 C48 1 0.607352 0.421021 0.141064 11.00000 0.03021 0.01939 = 0.02286 0.01159 0.00703 0.00720 AFIX 137 H48A 2 0.539913 0.422725 0.171184 11.00000 -1.50000 H48B 2 0.605238 0.454206 0.109803 11.00000 -1.50000 H48C 2 0.676266 0.443035 0.178746 11.00000 -1.50000 AFIX 0 C49 1 0.500925 0.297888 0.024409 11.00000 0.02100 0.02986 = 0.01895 0.01314 0.00265 0.00507 AFIX 137 H49A 2 0.504544 0.242423 -0.014469 11.00000 -1.50000 H49B 2 0.496560 0.333376 -0.004149 11.00000 -1.50000 H49C 2 0.433219 0.295804 0.053728 11.00000 -1.50000 AFIX 0 C50 1 0.714496 0.331361 0.037482 11.00000 0.02269 0.02929 = 0.02441 0.01496 0.00980 0.00527 AFIX 137 H50A 2 0.783119 0.354233 0.075454 11.00000 -1.50000 H50B 2 0.711389 0.364417 0.006190 11.00000 -1.50000 H50C 2 0.716647 0.274701 0.001005 11.00000 -1.50000 AFIX 0 C51 1 0.806522 0.402346 0.306255 11.00000 0.01407 0.04098 = 0.02481 0.01275 0.00457 -0.00517 AFIX 23 H51A 2 0.811228 0.350092 0.260701 11.00000 -1.20000 H51B 2 0.822633 0.446925 0.287147 11.00000 -1.20000 AFIX 0 C52 1 0.893597 0.418229 0.372855 11.00000 0.01771 0.06299 = 0.03297 0.01942 0.00480 0.01024 AFIX 137 H52A 2 0.885603 0.467926 0.419377 11.00000 -1.50000 H52B 2 0.969948 0.425792 0.354959 11.00000 -1.50000 H52C 2 0.882576 0.371427 0.388082 11.00000 -1.50000 AFIX 0 GE61 5 0.347211 0.282734 0.243972 11.00000 0.01178 0.01431 = 0.01443 0.00609 0.00335 0.00309 SE61 6 0.287991 0.367688 0.186460 11.00000 0.02131 0.02849 = 0.02647 0.01888 0.01038 0.01189 SI61 4 0.203717 0.204118 0.309808 11.00000 0.01296 0.01914 = 0.02177 0.01083 0.00475 0.00257 N61 3 0.289671 0.300990 0.342495 11.00000 0.01589 0.01914 = 0.01336 0.00396 0.00652 0.00470 N62 3 0.252245 0.181544 0.214921 11.00000 0.01441 0.01257 = 0.01474 0.00355 0.00228 -0.00084 C61 1 0.046628 0.200708 0.312411 11.00000 0.01594 0.03165 = 0.03214 0.01641 0.00922 0.00459 AFIX 137 H61A 2 0.023825 0.234865 0.286619 11.00000 -1.50000 H61B 2 0.027961 0.221537 0.368436 11.00000 -1.50000 H61C 2 0.005826 0.143937 0.283539 11.00000 -1.50000 AFIX 0 C62 1 0.236079 0.140688 0.363853 11.00000 0.02238 0.03215 = 0.03887 0.02548 0.00953 0.00531 AFIX 137 H62A 2 0.194306 0.084167 0.335125 11.00000 -1.50000 H62B 2 0.212855 0.163454 0.418625 11.00000 -1.50000 H62C 2 0.318102 0.141072 0.366242 11.00000 -1.50000 AFIX 0 C63 1 0.322099 0.367489 0.423188 11.00000 0.02216 0.02652 = 0.01572 0.00692 0.00637 0.00745 C64 1 0.217330 0.372194 0.471443 11.00000 0.02304 0.03889 = 0.02255 0.00551 0.00726 0.00735 AFIX 137 H64A 2 0.155755 0.383751 0.443946 11.00000 -1.50000 H64B 2 0.237358 0.416122 0.525453 11.00000 -1.50000 H64C 2 0.192025 0.319711 0.475722 11.00000 -1.50000 AFIX 0 C65 1 0.418332 0.350113 0.466994 11.00000 0.02107 0.03361 = 0.01854 0.01072 0.00468 0.00488 AFIX 137 H65A 2 0.393045 0.297911 0.471835 11.00000 -1.50000 H65B 2 0.438094 0.394473 0.520786 11.00000 -1.50000 H65C 2 0.485348 0.346854 0.436351 11.00000 -1.50000 AFIX 0 C66 1 0.359646 0.449148 0.416014 11.00000 0.02649 0.02160 = 0.02320 0.00460 0.00304 0.00556 AFIX 137 H66A 2 0.426196 0.446539 0.384957 11.00000 -1.50000 H66B 2 0.379604 0.493340 0.469884 11.00000 -1.50000 H66C 2 0.297247 0.459997 0.388595 11.00000 -1.50000 AFIX 0 C67 1 0.213090 0.116576 0.134557 11.00000 0.01684 0.01751 = 0.02001 0.00336 0.00025 0.00115 C68 1 0.104798 0.130732 0.100050 11.00000 0.02326 0.04416 = 0.02768 0.00131 -0.00465 0.01095 AFIX 137 H68A 2 0.043643 0.129120 0.134945 11.00000 -1.50000 H68B 2 0.081510 0.087659 0.045942 11.00000 -1.50000 H68C 2 0.120053 0.184463 0.097215 11.00000 -1.50000 AFIX 0 C69 1 0.188614 0.033864 0.141116 11.00000 0.04044 0.02176 = 0.03474 0.00533 0.00117 -0.00407 AFIX 137 H69A 2 0.258046 0.024661 0.162698 11.00000 -1.50000 H69B 2 0.163519 -0.010011 0.087679 11.00000 -1.50000 H69C 2 0.128573 0.033866 0.177178 11.00000 -1.50000 AFIX 0 C70 1 0.306448 0.116144 0.078440 11.00000 0.02621 0.02725 = 0.01779 -0.00038 0.00425 0.00214 AFIX 137 H70A 2 0.321035 0.168594 0.072935 11.00000 -1.50000 H70B 2 0.282028 0.071266 0.025474 11.00000 -1.50000 H70C 2 0.376344 0.108293 0.100809 11.00000 -1.50000 AFIX 0 C71 1 0.136524 0.367854 0.228091 11.00000 0.01961 0.03040 = 0.02442 0.01499 0.00896 0.01131 AFIX 23 H71A 2 0.103450 0.312305 0.224368 11.00000 -1.20000 H71B 2 0.144317 0.406522 0.285438 11.00000 -1.20000 AFIX 0 C72 1 0.058731 0.392938 0.180467 11.00000 0.01851 0.03713 = 0.03202 0.02174 0.00477 0.00711 AFIX 137 H72A 2 0.092535 0.447363 0.183146 11.00000 -1.50000 H72B 2 -0.015206 0.394801 0.202924 11.00000 -1.50000 H72C 2 0.048077 0.353026 0.124241 11.00000 -1.50000 AFIX 0 HKLF 4 REM pst_074m in P-1 REM R1 = 0.0382 for 12899 Fo > 4sig(Fo) and 0.0630 for all 17182 data REM 649 parameters refined using 0 restraints END WGHT 0.0378 7.4012 REM Highest difference peak 2.720, deepest hole -0.702, 1-sigma level 0.118 Q1 1 0.3745 0.2438 0.2808 11.00000 0.05 2.72 Q2 1 0.0139 0.7644 0.2238 11.00000 0.05 2.45 Q3 1 0.4007 0.1766 0.3655 11.00000 0.05 2.15 Q4 1 0.0763 0.8439 0.1471 11.00000 0.05 2.08 Q5 1 0.1801 0.2845 0.2596 11.00000 0.05 1.09 Q6 1 0.5705 0.2457 0.2204 11.00000 0.05 0.89 Q7 1 -0.2031 0.7272 0.2454 11.00000 0.05 0.83 Q8 1 0.1175 0.7287 0.2727 11.00000 0.05 0.82 Q9 1 0.6679 0.3528 0.3327 11.00000 0.05 0.79 Q10 1 -0.1360 0.6965 0.3485 11.00000 0.05 0.78 Q11 1 -0.0611 0.7692 0.2635 11.00000 0.05 0.77 ; _shelx_res_checksum 73573 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 Se1 Se 0.20649(3) 0.60449(2) 0.16401(2) 0.01668(8) Uani 1 1 d . . Ge1 Ge 0.17353(3) 0.72053(2) 0.27596(2) 0.01197(8) Uani 1 1 d . . Si1 Si 0.33514(8) 0.81791(6) 0.39067(6) 0.0191(2) Uani 1 1 d . . N1 N 0.2800(2) 0.81582(17) 0.30095(18) 0.0165(6) Uani 1 1 d . . N2 N 0.2367(2) 0.72889(18) 0.37318(17) 0.0179(6) Uani 1 1 d . . C1 C 0.4898(3) 0.8114(3) 0.3942(3) 0.0296(9) Uani 1 1 d . . H1A H 0.5030 0.7647 0.3463 0.044 Uiso 1 1 calc R U H1B H 0.5112 0.8039 0.4426 0.044 Uiso 1 1 calc R U H1C H 0.5360 0.8622 0.3953 0.044 Uiso 1 1 calc R U C2 C 0.3224(4) 0.9089(3) 0.4842(2) 0.0319(10) Uani 1 1 d . . H2A H 0.3713 0.9581 0.4839 0.048 Uiso 1 1 calc R U H2B H 0.3461 0.9000 0.5314 0.048 Uiso 1 1 calc R U H2C H 0.2430 0.9162 0.4863 0.048 Uiso 1 1 calc R U C3 C 0.3180(3) 0.8592(2) 0.2500(2) 0.0216(8) Uani 1 1 d . . C4 C 0.3652(4) 0.9488(2) 0.3034(3) 0.0340(10) Uani 1 1 d . . H4A H 0.3069 0.9725 0.3377 0.051 Uiso 1 1 calc R U H4B H 0.3866 0.9790 0.2698 0.051 Uiso 1 1 calc R U H4C H 0.4324 0.9528 0.3373 0.051 Uiso 1 1 calc R U C5 C 0.2158(3) 0.8547(3) 0.1953(3) 0.0281(9) Uani 1 1 d . . H5A H 0.1844 0.7971 0.1604 0.042 Uiso 1 1 calc R U H5B H 0.2406 0.8847 0.1620 0.042 Uiso 1 1 calc R U H5C H 0.1572 0.8793 0.2284 0.042 Uiso 1 1 calc R U C6 C 0.4088(3) 0.8206(3) 0.1971(3) 0.0306(10) Uani 1 1 d . . H6A H 0.4751 0.8239 0.2315 0.046 Uiso 1 1 calc R U H6B H 0.4321 0.8502 0.1633 0.046 Uiso 1 1 calc R U H6C H 0.3773 0.7629 0.1629 0.046 Uiso 1 1 calc R U C7 C 0.2050(3) 0.6827(2) 0.4232(2) 0.0230(8) Uani 1 1 d . . C8 C 0.1207(3) 0.7222(3) 0.4826(2) 0.0279(9) Uani 1 1 d . . H8A H 0.1553 0.7793 0.5167 0.042 Uiso 1 1 calc R U H8B H 0.1021 0.6918 0.5164 0.042 Uiso 1 1 calc R U H8C H 0.0509 0.7206 0.4526 0.042 Uiso 1 1 calc R U C9 C 0.1534(3) 0.5936(2) 0.3704(2) 0.0276(9) Uani 1 1 d . . H9A H 0.0845 0.5911 0.3390 0.041 Uiso 1 1 calc R U H9B H 0.1337 0.5636 0.4044 0.041 Uiso 1 1 calc R U H9C H 0.2087 0.5687 0.3339 0.041 Uiso 1 1 calc R U C10 C 0.3143(4) 0.6860(3) 0.4714(3) 0.0338(10) Uani 1 1 d . . H10A H 0.3686 0.6606 0.4341 0.051 Uiso 1 1 calc R U H10B H 0.2954 0.6561 0.5056 0.051 Uiso 1 1 calc R U H10C H 0.3485 0.7433 0.5051 0.051 Uiso 1 1 calc R U C11 C 0.3612(3) 0.6026(3) 0.2007(2) 0.0236(8) Uani 1 1 d . . H11A H 0.3947 0.6567 0.2439 0.028 Uiso 1 1 calc R U H11B H 0.3573 0.5607 0.2232 0.028 Uiso 1 1 calc R U C12 C 0.4363(3) 0.5833(3) 0.1324(3) 0.0338(10) Uani 1 1 d . . H12A H 0.3992 0.5328 0.0873 0.051 Uiso 1 1 calc R U H12B H 0.5097 0.5760 0.1505 0.051 Uiso 1 1 calc R U H12C H 0.4489 0.6287 0.1151 0.051 Uiso 1 1 calc R U Ge21 Ge -0.03120(3) 0.72391(2) 0.25315(2) 0.01297(8) Uani 1 1 d . . Se21 Se -0.13127(3) 0.64476(3) 0.31674(2) 0.02301(9) Uani 1 1 d . . Si21 Si -0.13646(8) 0.79689(6) 0.18032(6) 0.0178(2) Uani 1 1 d . . N21 N -0.1015(2) 0.70055(18) 0.15288(17) 0.0153(6) Uani 1 1 d . . N22 N -0.0715(2) 0.82489(18) 0.27629(18) 0.0178(6) Uani 1 1 d . . C21 C -0.2925(3) 0.7990(3) 0.1760(3) 0.0274(9) Uani 1 1 d . . H21A H -0.3320 0.7647 0.2016 0.041 Uiso 1 1 calc R U H21B H -0.3235 0.7778 0.1197 0.041 Uiso 1 1 calc R U H21C H -0.3036 0.8556 0.2045 0.041 Uiso 1 1 calc R U C22 C -0.0733(3) 0.8567(3) 0.1221(3) 0.0318(10) Uani 1 1 d . . H22A H -0.0880 0.9127 0.1468 0.048 Uiso 1 1 calc R U H22B H -0.1080 0.8301 0.0664 0.048 Uiso 1 1 calc R U H22C H 0.0091 0.8587 0.1226 0.048 Uiso 1 1 calc R U C23 C -0.1070(3) 0.6317(2) 0.0744(2) 0.0208(8) Uani 1 1 d . . C24 C -0.2160(3) 0.6241(3) 0.0239(2) 0.0337(10) Uani 1 1 d . . H24A H -0.2825 0.6164 0.0527 0.051 Uiso 1 1 calc R U H24B H -0.2221 0.5769 -0.0280 0.051 Uiso 1 1 calc R U H24C H -0.2128 0.6742 0.0147 0.051 Uiso 1 1 calc R U C25 C -0.1119(3) 0.5519(2) 0.0859(2) 0.0255(8) Uani 1 1 d . . H25A H -0.0428 0.5560 0.1182 0.038 Uiso 1 1 calc R U H25B H -0.1171 0.5058 0.0333 0.038 Uiso 1 1 calc R U H25C H -0.1789 0.5427 0.1138 0.038 Uiso 1 1 calc R U C26 C -0.0030(3) 0.6452(3) 0.0300(2) 0.0275(9) Uani 1 1 d . . H26A H -0.0009 0.6954 0.0212 0.041 Uiso 1 1 calc R U H26B H -0.0080 0.5983 -0.0219 0.041 Uiso 1 1 calc R U H26C H 0.0665 0.6506 0.0625 0.041 Uiso 1 1 calc R U C27 C -0.0702(3) 0.8931(2) 0.3539(2) 0.0243(8) Uani 1 1 d . . C28 C -0.1772(4) 0.8789(3) 0.3955(3) 0.0363(11) Uani 1 1 d . . H28A H -0.2450 0.8744 0.3618 0.054 Uiso 1 1 calc R U H28B H -0.1738 0.9252 0.4478 0.054 Uiso 1 1 calc R U H28C H -0.1813 0.8281 0.4035 0.054 Uiso 1 1 calc R U C29 C -0.0649(4) 0.9721(3) 0.3402(3) 0.0369(11) Uani 1 1 d . . H29A H 0.0014 0.9798 0.3112 0.055 Uiso 1 1 calc R U H29B H -0.0581 1.0192 0.3923 0.055 Uiso 1 1 calc R U H29C H -0.1345 0.9678 0.3084 0.055 Uiso 1 1 calc R U C30 C 0.0358(3) 0.9020(3) 0.4068(2) 0.0301(10) Uani 1 1 d . . H30A H 0.0325 0.8521 0.4163 0.045 Uiso 1 1 calc R U H30B H 0.0391 0.9492 0.4584 0.045 Uiso 1 1 calc R U H30C H 0.1039 0.9106 0.3797 0.045 Uiso 1 1 calc R U C31 C -0.2853(3) 0.6452(2) 0.2775(2) 0.0204(8) Uani 1 1 d . . H31A H -0.2912 0.7014 0.2844 0.025 Uiso 1 1 calc R U H31B H -0.3007 0.6087 0.2196 0.025 Uiso 1 1 calc R U C32 C -0.3718(3) 0.6156(3) 0.3249(2) 0.0258(9) Uani 1 1 d . . H32A H -0.3607 0.5621 0.3221 0.039 Uiso 1 1 calc R U H32B H -0.4490 0.6102 0.3020 0.039 Uiso 1 1 calc R U H32C H -0.3616 0.6552 0.3812 0.039 Uiso 1 1 calc R U Se41 Se 0.65126(3) 0.39595(2) 0.34152(2) 0.01675(8) Uani 1 1 d . . Ge41 Ge 0.55373(3) 0.28501(2) 0.22479(2) 0.01231(8) Uani 1 1 d . . Si41 Si 0.66008(8) 0.19089(6) 0.10787(6) 0.0159(2) Uani 1 1 d . . N41 N 0.6050(2) 0.18689(17) 0.19452(17) 0.0148(6) Uani 1 1 d . . N42 N 0.6144(2) 0.28262(18) 0.13050(17) 0.0160(6) Uani 1 1 d . . C41 C 0.5955(3) 0.1065(2) 0.0101(2) 0.0234(8) Uani 1 1 d . . H41A H 0.5131 0.1040 0.0053 0.035 Uiso 1 1 calc R U H41B H 0.6103 0.0541 0.0081 0.035 Uiso 1 1 calc R U H41C H 0.6292 0.1171 -0.0343 0.035 Uiso 1 1 calc R U C42 C 0.8171(3) 0.1946(3) 0.1069(3) 0.0269(9) Uani 1 1 d . . H42A H 0.8440 0.2060 0.0612 0.040 Uiso 1 1 calc R U H42B H 0.8335 0.1417 0.1020 0.040 Uiso 1 1 calc R U H42C H 0.8561 0.2381 0.1572 0.040 Uiso 1 1 calc R U C43 C 0.6177(3) 0.1383(2) 0.2412(2) 0.0186(7) Uani 1 1 d . . C44 C 0.6039(4) 0.0480(2) 0.1835(3) 0.0292(9) Uani 1 1 d . . H44A H 0.5304 0.0304 0.1511 0.044 Uiso 1 1 calc R U H44B H 0.6068 0.0146 0.2144 0.044 Uiso 1 1 calc R U H44C H 0.6656 0.0413 0.1479 0.044 Uiso 1 1 calc R U C45 C 0.5246(3) 0.1474(2) 0.2991(2) 0.0234(8) Uani 1 1 d . . H45A H 0.5323 0.2053 0.3359 0.035 Uiso 1 1 calc R U H45B H 0.5322 0.1147 0.3302 0.035 Uiso 1 1 calc R U H45C H 0.4496 0.1281 0.2684 0.035 Uiso 1 1 calc R U C46 C 0.7348(3) 0.1678(3) 0.2903(3) 0.0303(9) Uani 1 1 d . . H46A H 0.7952 0.1609 0.2536 0.045 Uiso 1 1 calc R U H46B H 0.7406 0.1355 0.3220 0.045 Uiso 1 1 calc R U H46C H 0.7434 0.2259 0.3265 0.045 Uiso 1 1 calc R U C47 C 0.6083(3) 0.3325(2) 0.0842(2) 0.0187(7) Uani 1 1 d . . C48 C 0.6074(3) 0.4210(2) 0.1411(2) 0.0228(8) Uani 1 1 d . . H48A H 0.5399 0.4227 0.1712 0.034 Uiso 1 1 calc R U H48B H 0.6052 0.4542 0.1098 0.034 Uiso 1 1 calc R U H48C H 0.6763 0.4430 0.1787 0.034 Uiso 1 1 calc R U C49 C 0.5009(3) 0.2979(2) 0.0244(2) 0.0222(8) Uani 1 1 d . . H49A H 0.5045 0.2424 -0.0145 0.033 Uiso 1 1 calc R U H49B H 0.4966 0.3334 -0.0041 0.033 Uiso 1 1 calc R U H49C H 0.4332 0.2958 0.0537 0.033 Uiso 1 1 calc R U C50 C 0.7145(3) 0.3314(2) 0.0375(2) 0.0240(8) Uani 1 1 d . . H50A H 0.7831 0.3542 0.0755 0.036 Uiso 1 1 calc R U H50B H 0.7114 0.3644 0.0062 0.036 Uiso 1 1 calc R U H50C H 0.7166 0.2747 0.0010 0.036 Uiso 1 1 calc R U C51 C 0.8065(3) 0.4023(3) 0.3063(2) 0.0281(9) Uani 1 1 d . . H51A H 0.8112 0.3501 0.2607 0.034 Uiso 1 1 calc R U H51B H 0.8226 0.4469 0.2871 0.034 Uiso 1 1 calc R U C52 C 0.8936(3) 0.4182(3) 0.3729(3) 0.0376(11) Uani 1 1 d . . H52A H 0.8856 0.4679 0.4194 0.056 Uiso 1 1 calc R U H52B H 0.9699 0.4258 0.3550 0.056 Uiso 1 1 calc R U H52C H 0.8826 0.3714 0.3881 0.056 Uiso 1 1 calc R U Ge61 Ge 0.34721(3) 0.28273(2) 0.24397(2) 0.01333(8) Uani 1 1 d . . Se61 Se 0.28799(3) 0.36769(2) 0.18646(2) 0.02193(9) Uani 1 1 d . . Si61 Si 0.20372(8) 0.20412(6) 0.30981(6) 0.0172(2) Uani 1 1 d . . N61 N 0.2897(2) 0.30099(18) 0.34249(17) 0.0167(6) Uani 1 1 d . . N62 N 0.2522(2) 0.18154(17) 0.21492(17) 0.0150(6) Uani 1 1 d . . C61 C 0.0466(3) 0.2007(3) 0.3124(2) 0.0254(8) Uani 1 1 d . . H61A H 0.0238 0.2349 0.2866 0.038 Uiso 1 1 calc R U H61B H 0.0280 0.2215 0.3684 0.038 Uiso 1 1 calc R U H61C H 0.0058 0.1439 0.2835 0.038 Uiso 1 1 calc R U C62 C 0.2361(3) 0.1407(3) 0.3639(3) 0.0275(9) Uani 1 1 d . . H62A H 0.1943 0.0842 0.3351 0.041 Uiso 1 1 calc R U H62B H 0.2129 0.1635 0.4186 0.041 Uiso 1 1 calc R U H62C H 0.3181 0.1411 0.3662 0.041 Uiso 1 1 calc R U C63 C 0.3221(3) 0.3675(2) 0.4232(2) 0.0216(8) Uani 1 1 d . . C64 C 0.2173(3) 0.3722(3) 0.4714(2) 0.0302(9) Uani 1 1 d . . H64A H 0.1558 0.3838 0.4439 0.045 Uiso 1 1 calc R U H64B H 0.2374 0.4161 0.5255 0.045 Uiso 1 1 calc R U H64C H 0.1920 0.3197 0.4757 0.045 Uiso 1 1 calc R U C65 C 0.4183(3) 0.3501(3) 0.4670(2) 0.0244(8) Uani 1 1 d . . H65A H 0.3930 0.2979 0.4718 0.037 Uiso 1 1 calc R U H65B H 0.4381 0.3945 0.5208 0.037 Uiso 1 1 calc R U H65C H 0.4853 0.3469 0.4364 0.037 Uiso 1 1 calc R U C66 C 0.3596(3) 0.4491(2) 0.4160(2) 0.0251(8) Uani 1 1 d . . H66A H 0.4262 0.4465 0.3850 0.038 Uiso 1 1 calc R U H66B H 0.3796 0.4933 0.4699 0.038 Uiso 1 1 calc R U H66C H 0.2972 0.4600 0.3886 0.038 Uiso 1 1 calc R U C67 C 0.2131(3) 0.1166(2) 0.1346(2) 0.0198(8) Uani 1 1 d . . C68 C 0.1048(3) 0.1307(3) 0.1000(3) 0.0355(11) Uani 1 1 d . . H68A H 0.0436 0.1291 0.1349 0.053 Uiso 1 1 calc R U H68B H 0.0815 0.0877 0.0459 0.053 Uiso 1 1 calc R U H68C H 0.1201 0.1845 0.0972 0.053 Uiso 1 1 calc R U C69 C 0.1886(4) 0.0339(3) 0.1411(3) 0.0356(10) Uani 1 1 d . . H69A H 0.2580 0.0247 0.1627 0.053 Uiso 1 1 calc R U H69B H 0.1635 -0.0100 0.0877 0.053 Uiso 1 1 calc R U H69C H 0.1286 0.0339 0.1772 0.053 Uiso 1 1 calc R U C70 C 0.3064(3) 0.1161(3) 0.0784(2) 0.0272(9) Uani 1 1 d . . H70A H 0.3210 0.1686 0.0729 0.041 Uiso 1 1 calc R U H70B H 0.2820 0.0713 0.0255 0.041 Uiso 1 1 calc R U H70C H 0.3763 0.1083 0.1008 0.041 Uiso 1 1 calc R U C71 C 0.1365(3) 0.3679(3) 0.2281(2) 0.0227(8) Uani 1 1 d . . H71A H 0.1034 0.3123 0.2244 0.027 Uiso 1 1 calc R U H71B H 0.1443 0.4065 0.2854 0.027 Uiso 1 1 calc R U C72 C 0.0587(3) 0.3929(3) 0.1805(2) 0.0265(9) Uani 1 1 d . . H72A H 0.0925 0.4474 0.1831 0.040 Uiso 1 1 calc R U H72B H -0.0152 0.3948 0.2029 0.040 Uiso 1 1 calc R U H72C H 0.0481 0.3530 0.1242 0.040 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 Se1 0.01529(17) 0.01538(18) 0.01582(17) 0.00168(14) 0.00106(13) 0.00551(14) Ge1 0.01067(16) 0.01237(18) 0.01203(17) 0.00378(14) 0.00104(13) 0.00301(13) Si1 0.0134(5) 0.0179(5) 0.0200(5) 0.0017(4) -0.0032(4) 0.0030(4) N1 0.0155(14) 0.0107(15) 0.0197(15) 0.0039(12) 0.0012(12) -0.0015(12) N2 0.0189(15) 0.0186(16) 0.0141(14) 0.0058(13) -0.0035(12) 0.0008(12) C1 0.0175(19) 0.026(2) 0.039(2) 0.0072(19) -0.0053(17) 0.0041(17) C2 0.027(2) 0.026(2) 0.029(2) -0.0021(18) -0.0062(17) 0.0026(18) C3 0.0159(17) 0.020(2) 0.032(2) 0.0150(17) 0.0047(15) 0.0022(15) C4 0.031(2) 0.021(2) 0.047(3) 0.014(2) 0.004(2) -0.0025(18) C5 0.0194(19) 0.037(2) 0.039(2) 0.026(2) 0.0058(17) 0.0064(17) C6 0.025(2) 0.037(3) 0.040(2) 0.023(2) 0.0165(18) 0.0114(19) C7 0.0200(18) 0.032(2) 0.0218(19) 0.0159(18) 0.0020(15) 0.0066(16) C8 0.026(2) 0.041(3) 0.021(2) 0.0165(19) 0.0039(16) 0.0085(19) C9 0.033(2) 0.028(2) 0.031(2) 0.0197(19) 0.0073(18) 0.0088(18) C10 0.031(2) 0.051(3) 0.028(2) 0.025(2) -0.0033(18) 0.010(2) C11 0.0205(18) 0.030(2) 0.0225(19) 0.0101(17) 0.0030(15) 0.0120(17) C12 0.0186(19) 0.052(3) 0.036(2) 0.019(2) 0.0085(17) 0.017(2) Ge21 0.01135(16) 0.01394(18) 0.01201(17) 0.00375(15) 0.00109(13) 0.00207(14) Se21 0.01509(17) 0.0338(2) 0.0264(2) 0.02040(18) 0.00062(14) 0.00056(16) Si21 0.0149(5) 0.0188(5) 0.0210(5) 0.0091(4) 0.0009(4) 0.0043(4) N21 0.0151(14) 0.0176(16) 0.0115(14) 0.0032(12) -0.0021(11) 0.0058(12) N22 0.0156(14) 0.0135(15) 0.0196(15) 0.0005(13) 0.0009(12) 0.0064(12) C21 0.0182(18) 0.028(2) 0.035(2) 0.0105(19) -0.0025(16) 0.0081(17) C22 0.028(2) 0.037(3) 0.044(3) 0.030(2) 0.0007(19) 0.0079(19) C23 0.0169(17) 0.025(2) 0.0139(17) -0.0005(15) -0.0017(14) 0.0072(15) C24 0.029(2) 0.041(3) 0.021(2) 0.0000(19) -0.0069(17) 0.012(2) C25 0.0237(19) 0.019(2) 0.024(2) -0.0012(16) 0.0020(16) 0.0024(16) C26 0.030(2) 0.035(2) 0.0178(19) 0.0080(18) 0.0044(16) 0.0140(19) C27 0.0184(18) 0.018(2) 0.024(2) -0.0054(16) 0.0008(15) 0.0056(15) C28 0.026(2) 0.035(3) 0.030(2) -0.006(2) 0.0100(18) 0.0083(19) C29 0.038(2) 0.019(2) 0.043(3) 0.001(2) -0.003(2) 0.0100(19) C30 0.026(2) 0.028(2) 0.023(2) -0.0067(17) -0.0039(16) 0.0111(18) C31 0.0157(17) 0.027(2) 0.0225(19) 0.0151(17) 0.0018(14) 0.0015(15) C32 0.0163(18) 0.038(2) 0.028(2) 0.0178(19) 0.0055(15) 0.0056(17) Se41 0.01439(16) 0.01729(18) 0.01323(16) 0.00230(14) 0.00233(13) -0.00107(14) Ge41 0.01023(16) 0.01295(18) 0.01185(17) 0.00350(14) 0.00283(13) 0.00101(14) Si41 0.0134(4) 0.0149(5) 0.0172(5) 0.0035(4) 0.0059(4) 0.0040(4) N41 0.0182(14) 0.0122(15) 0.0147(14) 0.0057(12) 0.0018(11) 0.0039(12) N42 0.0183(14) 0.0165(15) 0.0130(14) 0.0051(12) 0.0070(11) 0.0042(12) C41 0.030(2) 0.018(2) 0.0193(18) 0.0033(16) 0.0086(16) 0.0071(16) C42 0.0193(19) 0.028(2) 0.033(2) 0.0110(19) 0.0088(16) 0.0067(17) C43 0.0210(18) 0.0143(18) 0.0215(18) 0.0085(15) 0.0012(14) 0.0028(15) C44 0.042(2) 0.018(2) 0.029(2) 0.0096(18) 0.0048(18) 0.0110(18) C45 0.0246(19) 0.020(2) 0.028(2) 0.0129(17) 0.0023(16) 0.0012(16) C46 0.0194(19) 0.043(3) 0.036(2) 0.024(2) -0.0019(17) 0.0059(18) C47 0.0204(18) 0.0185(19) 0.0180(18) 0.0084(15) 0.0053(14) 0.0032(15) C48 0.030(2) 0.019(2) 0.0229(19) 0.0116(17) 0.0070(16) 0.0072(16) C49 0.0210(18) 0.030(2) 0.0189(18) 0.0131(17) 0.0027(15) 0.0051(16) C50 0.0227(19) 0.029(2) 0.024(2) 0.0150(18) 0.0098(16) 0.0053(17) C51 0.0141(18) 0.041(3) 0.025(2) 0.0128(19) 0.0046(15) -0.0052(17) C52 0.018(2) 0.063(3) 0.033(2) 0.019(2) 0.0048(17) 0.010(2) Ge61 0.01178(16) 0.01431(19) 0.01443(17) 0.00609(15) 0.00335(13) 0.00309(14) Se61 0.02131(18) 0.0285(2) 0.0265(2) 0.01888(17) 0.01038(15) 0.01189(16) Si61 0.0130(4) 0.0191(5) 0.0218(5) 0.0108(4) 0.0048(4) 0.0026(4) N61 0.0159(14) 0.0191(16) 0.0134(14) 0.0040(12) 0.0065(11) 0.0047(12) N62 0.0144(14) 0.0126(15) 0.0147(14) 0.0036(12) 0.0023(11) -0.0008(12) C61 0.0159(18) 0.032(2) 0.032(2) 0.0164(19) 0.0092(16) 0.0046(16) C62 0.0224(19) 0.032(2) 0.039(2) 0.025(2) 0.0095(17) 0.0053(17) C63 0.0222(18) 0.027(2) 0.0157(17) 0.0069(16) 0.0064(14) 0.0074(16) C64 0.023(2) 0.039(3) 0.023(2) 0.0055(19) 0.0073(16) 0.0073(18) C65 0.0211(19) 0.034(2) 0.0185(18) 0.0107(17) 0.0047(15) 0.0049(17) C66 0.026(2) 0.022(2) 0.023(2) 0.0046(17) 0.0030(16) 0.0056(17) C67 0.0168(17) 0.0175(19) 0.0200(18) 0.0034(15) 0.0002(14) 0.0011(15) C68 0.023(2) 0.044(3) 0.028(2) 0.001(2) -0.0047(17) 0.011(2) C69 0.040(3) 0.022(2) 0.035(2) 0.0053(19) 0.001(2) -0.0041(19) C70 0.026(2) 0.027(2) 0.0178(19) -0.0004(17) 0.0043(15) 0.0021(17) C71 0.0196(18) 0.030(2) 0.0244(19) 0.0150(18) 0.0090(15) 0.0113(16) C72 0.0185(18) 0.037(2) 0.032(2) 0.022(2) 0.0048(16) 0.0071(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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 C11 Se1 Ge1 98.55(11) N1 Ge1 N2 81.75(13) N1 Ge1 Se1 115.59(9) N2 Ge1 Se1 113.45(10) N1 Ge1 Ge21 118.46(9) N2 Ge1 Ge21 122.29(9) Se1 Ge1 Ge21 104.764(18) Se1 Ge1 Si1 122.81(3) Ge21 Ge1 Si1 132.41(3) N1 Si1 N2 88.40(14) N1 Si1 C2 116.47(18) N2 Si1 C2 115.46(18) N1 Si1 C1 114.50(18) N2 Si1 C1 117.16(17) C2 Si1 C1 104.94(19) C2 Si1 Ge1 128.17(13) C1 Si1 Ge1 126.88(14) C3 N1 Si1 134.1(2) C3 N1 Ge1 129.3(2) Si1 N1 Ge1 95.04(14) C7 N2 Si1 132.2(2) C7 N2 Ge1 132.5(2) Si1 N2 Ge1 94.81(14) N1 C3 C4 108.9(3) N1 C3 C6 111.1(3) C4 C3 C6 110.3(3) N1 C3 C5 109.2(3) C4 C3 C5 108.6(3) C6 C3 C5 108.7(3) N2 C7 C9 110.4(3) N2 C7 C8 110.4(3) C9 C7 C8 110.3(3) N2 C7 C10 107.9(3) C9 C7 C10 109.0(3) C8 C7 C10 108.8(3) C12 C11 Se1 111.0(3) N21 Ge21 N22 81.97(13) N21 Ge21 Se21 112.17(9) N22 Ge21 Se21 115.38(9) N21 Ge21 Ge1 123.10(9) N22 Ge21 Ge1 118.28(9) Se21 Ge21 Ge1 105.228(18) Se21 Ge21 Si21 122.03(3) Ge1 Ge21 Si21 132.72(3) C31 Se21 Ge21 96.55(10) N22 Si21 N21 88.64(14) N22 Si21 C21 114.86(17) N21 Si21 C21 115.97(17) N22 Si21 C22 116.71(18) N21 Si21 C22 115.41(17) C21 Si21 C22 105.25(19) C21 Si21 Ge21 126.61(14) C22 Si21 Ge21 128.15(13) C23 N21 Si21 131.8(2) C23 N21 Ge21 132.6(2) Si21 N21 Ge21 94.77(14) C27 N22 Si21 134.5(2) C27 N22 Ge21 129.4(3) Si21 N22 Ge21 94.62(14) N21 C23 C26 110.8(3) N21 C23 C25 109.7(3) C26 C23 C25 109.3(3) N21 C23 C24 108.8(3) C26 C23 C24 109.4(3) C25 C23 C24 108.7(3) N22 C27 C30 108.8(3) N22 C27 C28 111.1(3) C30 C27 C28 109.8(4) N22 C27 C29 108.6(3) C30 C27 C29 109.1(3) C28 C27 C29 109.4(3) C32 C31 Se21 109.1(2) C51 Se41 Ge41 99.09(12) N41 Ge41 N42 81.78(12) N41 Ge41 Se41 116.26(9) N42 Ge41 Se41 112.79(9) N41 Ge41 Ge61 117.93(9) N42 Ge41 Ge61 122.49(9) Se41 Ge41 Ge61 105.022(18) Se41 Ge41 Si41 122.99(3) Ge61 Ge41 Si41 131.98(3) N42 Si41 N41 88.87(13) N42 Si41 C41 114.78(16) N41 Si41 C41 116.66(16) N42 Si41 C42 116.86(17) N41 Si41 C42 114.09(17) C41 Si41 C42 105.54(18) C41 Si41 Ge41 127.75(12) C42 Si41 Ge41 126.70(14) C43 N41 Si41 134.3(2) C43 N41 Ge41 129.4(2) Si41 N41 Ge41 94.62(13) C47 N42 Si41 131.9(2) C47 N42 Ge41 132.6(2) Si41 N42 Ge41 94.72(14) N41 C43 C44 108.9(3) N41 C43 C45 109.1(3) C44 C43 C45 109.0(3) N41 C43 C46 111.0(3) C44 C43 C46 110.1(3) C45 C43 C46 108.8(3) N42 C47 C48 110.0(3) N42 C47 C50 108.7(3) C48 C47 C50 108.6(3) N42 C47 C49 110.7(3) C48 C47 C49 109.7(3) C50 C47 C49 109.2(3) C52 C51 Se41 111.4(3) N62 Ge61 N61 81.98(13) N62 Ge61 Se61 114.94(9) N61 Ge61 Se61 111.50(9) N62 Ge61 Ge41 117.70(9) N61 Ge61 Ge41 122.74(9) Se61 Ge61 Ge41 106.745(18) Se61 Ge61 Si61 121.69(3) Ge41 Ge61 Si61 131.55(3) C71 Se61 Ge61 96.03(11) N61 Si61 N62 88.59(14) N61 Si61 C62 115.18(17) N62 Si61 C62 117.29(17) N61 Si61 C61 116.27(17) N62 Si61 C61 114.63(16) C62 Si61 C61 104.97(17) C62 Si61 Ge61 127.88(12) C61 Si61 Ge61 127.14(13) C63 N61 Si61 132.2(2) C63 N61 Ge61 132.2(2) Si61 N61 Ge61 94.70(14) C67 N62 Si61 133.8(2) C67 N62 Ge61 129.8(2) Si61 N62 Ge61 94.72(14) N61 C63 C66 109.8(3) N61 C63 C65 110.5(3) C66 C63 C65 110.1(3) N61 C63 C64 108.3(3) C66 C63 C64 108.9(3) C65 C63 C64 109.1(3) N62 C67 C70 109.2(3) N62 C67 C69 108.8(3) C70 C67 C69 109.2(3) N62 C67 C68 110.9(3) C70 C67 C68 109.1(3) C69 C67 C68 109.5(3) C72 C71 Se61 110.2(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se1 C11 1.968(4) Se1 Ge1 2.3700(5) Ge1 N1 1.846(3) Ge1 N2 1.851(3) Ge1 Ge21 2.4921(5) Ge1 Si1 2.6414(11) Si1 N1 1.734(3) Si1 N2 1.736(3) Si1 C2 1.869(4) Si1 C1 1.875(4) N1 C3 1.467(5) N2 C7 1.476(5) C3 C4 1.519(6) C3 C6 1.533(5) C3 C5 1.534(5) C7 C9 1.520(6) C7 C8 1.536(5) C7 C10 1.542(5) C11 C12 1.506(5) Ge21 N21 1.851(3) Ge21 N22 1.856(3) Ge21 Se21 2.3650(5) Ge21 Si21 2.6438(10) Se21 C31 1.967(3) Si21 N22 1.740(3) Si21 N21 1.740(3) Si21 C21 1.874(4) Si21 C22 1.877(4) N21 C23 1.466(4) N22 C27 1.458(5) C23 C26 1.531(5) C23 C25 1.531(5) C23 C24 1.537(5) C27 C30 1.525(5) C27 C28 1.532(6) C27 C29 1.537(6) C31 C32 1.518(5) Se41 C51 1.974(4) Se41 Ge41 2.3725(5) Ge41 N41 1.854(3) Ge41 N42 1.859(3) Ge41 Ge61 2.4955(5) Ge41 Si41 2.6430(10) Si41 N42 1.731(3) Si41 N41 1.740(3) Si41 C41 1.866(4) Si41 C42 1.868(4) N41 C43 1.467(4) N42 C47 1.467(4) C43 C44 1.528(5) C43 C45 1.529(5) C43 C46 1.540(5) C47 C48 1.524(5) C47 C50 1.537(5) C47 C49 1.538(5) C51 C52 1.488(5) Ge61 N62 1.850(3) Ge61 N61 1.854(3) Ge61 Se61 2.3634(5) Ge61 Si61 2.6428(10) Se61 C71 1.974(3) Si61 N61 1.737(3) Si61 N62 1.742(3) Si61 C62 1.863(4) Si61 C61 1.871(4) N61 C63 1.473(5) N62 C67 1.470(4) C63 C66 1.526(5) C63 C65 1.534(5) C63 C64 1.536(5) C67 C70 1.523(5) C67 C69 1.527(6) C67 C68 1.534(5) C71 C72 1.501(5)