#------------------------------------------------------------------------------ #$Date: 2016-03-26 14:43:29 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180274 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116053.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_7116053 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 S2 Si2' _chemical_formula_sum 'C24 H58 Ge2 N4 S2 Si2' _chemical_formula_weight 668.22 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 109.874(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.9171(8) _cell_length_b 17.7348(12) _cell_length_c 17.6945(10) _cell_measurement_reflns_used 40556 _cell_measurement_temperature 180(1) _cell_measurement_theta_max 32.50 _cell_measurement_theta_min 2.30 _cell_volume 3517.0(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 'BRUKER AXS Inc. 2013 Vers. 2013/4' _computing_structure_refinement 'BRUKER AXS Inc. 2013 Vers. 2013/4' _computing_structure_solution 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _diffrn_ambient_temperature 180(1) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.984 _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 0.0634 _diffrn_reflns_av_unetI/netI 0.0506 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 81721 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.890 _diffrn_reflns_theta_min 1.817 _diffrn_source 'sealed X-RAY tube' _exptl_absorpt_coefficient_mu 1.915 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.56 _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 1.262 _exptl_crystal_description block _exptl_crystal_F_000 1416 _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.330 _exptl_crystal_size_min 0.270 _refine_diff_density_max 0.779 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 13009 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0594 _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^)+(0.0383P)^2^+14.8765P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1313 _refine_ls_wR_factor_ref 0.1467 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10491 _reflns_number_total 13009 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc07921c2.cif _cod_data_source_block pst_014s _cod_database_code 7116053 #BEGIN Tags that were not found in dictionaries: _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 0.530 _shelx_estimated_absorpt_t_max 0.626 _shelxl_version_number 2013-4 _shelx_res_file ; TITL pst_014s P 21 R = New: P21/c CELL 0.71073 11.9171 17.7348 17.6945 90.000 109.874 90.000 ZERR 4 0.0008 0.0012 0.0010 0.000 0.004 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N Ge S Si UNIT 96 232 16 8 8 8 OMIT 0 14 1 OMIT 0 17 4 OMIT -1 7 5 OMIT 7 1 3 OMIT -5 6 1 OMIT -14 11 7 OMIT -9 13 9 OMIT 0 8 6 OMIT -7 14 10 OMIT -1 0 -8 OMIT -6 4 6 OMIT -5 6 4 OMIT -8 2 3 OMIT -2 11 9 OMIT -14 4 11 OMIT 0 8 3 OMIT 0 18 5 OMIT -12 7 13 OMIT -14 6 10 OMIT -9 12 10 OMIT -6 7 1 OMIT 11 0 -14 OMIT 7 0 -18 OMIT -14 6 12 OMIT 15 1 1 OMIT -14 11 9 OMIT -8 22 8 TEMP -93 TWIN 1 0 0 0 -1 0 -1 0 -1 L.S. 15 FMAP 2 PLAN 10 SIZE 0.27 0.33 0.38 ACTA WGHT 0.038300 14.876495 BASF 0.22484 FVAR 0.08856 GE1 4 0.294263 0.329661 0.233511 11.00000 0.01990 0.01826 = 0.02499 0.00127 0.01004 0.00220 GE2 4 0.135279 0.391469 0.271611 11.00000 0.02424 0.02109 = 0.02573 0.00141 0.01172 0.00504 SI1 6 0.526223 0.348666 0.270205 11.00000 0.02175 0.02638 = 0.05185 0.00392 0.01368 0.00214 SI2 6 0.009334 0.516122 0.228052 11.00000 0.03727 0.02434 = 0.04261 0.00357 0.01852 0.01200 S1 5 0.195487 0.242102 0.145892 11.00000 0.03264 0.03201 = 0.04243 -0.01301 0.01108 0.00098 S2 5 0.110535 0.311693 0.362016 11.00000 0.03933 0.04309 = 0.04136 0.01876 0.02503 0.01771 N1 3 0.435443 0.295557 0.308567 11.00000 0.01926 0.02679 = 0.02796 0.00409 0.00471 0.00492 N2 3 0.398504 0.386556 0.200237 11.00000 0.02840 0.02636 = 0.04242 0.01332 0.01744 0.00684 N3 3 0.147734 0.492552 0.298352 11.00000 0.04011 0.02498 = 0.03325 -0.00606 0.01217 0.00942 N4 3 -0.006274 0.422708 0.195822 11.00000 0.02177 0.02273 = 0.03031 0.00328 0.00975 0.00577 C1 1 0.461701 0.245693 0.378060 11.00000 0.03140 0.03386 = 0.03166 0.00461 0.00860 0.00841 C2 1 0.462673 0.289376 0.452678 11.00000 0.06358 0.05475 = 0.03006 0.00322 0.01155 0.00901 AFIX 137 H2A 2 0.523141 0.329220 0.464126 11.00000 -1.50000 H2B 2 0.481470 0.254932 0.498622 11.00000 -1.50000 H2C 2 0.384029 0.312001 0.443161 11.00000 -1.50000 AFIX 0 C3 1 0.365912 0.183753 0.361522 11.00000 0.04961 0.03296 = 0.04326 0.01361 0.02292 0.00578 AFIX 137 H3A 2 0.287149 0.207082 0.349145 11.00000 -1.50000 H3B 2 0.382297 0.151631 0.409128 11.00000 -1.50000 H3C 2 0.367291 0.153103 0.315763 11.00000 -1.50000 AFIX 0 C4 1 0.584050 0.208686 0.394141 11.00000 0.03919 0.05814 = 0.06315 0.02380 0.00922 0.02305 AFIX 137 H4A 2 0.583557 0.180191 0.346575 11.00000 -1.50000 H4B 2 0.600984 0.174449 0.440147 11.00000 -1.50000 H4C 2 0.645732 0.247786 0.405967 11.00000 -1.50000 AFIX 0 C5 1 0.376371 0.440148 0.133428 11.00000 0.04461 0.02535 = 0.05019 0.01221 0.02986 0.00383 PART 1 C6 1 0.487013 0.494979 0.156114 10.75000 0.05733 AFIX 137 H6A 2 0.481655 0.526995 0.109874 10.75000 -1.50000 H6B 2 0.560740 0.465333 0.171007 10.75000 -1.50000 H6C 2 0.487421 0.526692 0.201562 10.75000 -1.50000 AFIX 0 C7 1 0.271022 0.487074 0.124616 10.75000 0.04151 AFIX 137 H7A 2 0.264975 0.526666 0.084785 10.75000 -1.50000 H7B 2 0.278689 0.510222 0.176427 10.75000 -1.50000 H7C 2 0.199154 0.455627 0.106759 10.75000 -1.50000 AFIX 0 C8 1 0.371380 0.399559 0.060054 10.75000 0.06635 AFIX 137 H8A 2 0.444515 0.369979 0.070265 10.75000 -1.50000 H8B 2 0.364059 0.435865 0.016883 10.75000 -1.50000 H8C 2 0.302232 0.365736 0.044028 10.75000 -1.50000 AFIX 0 PART 2 C6A 1 0.344200 0.512012 0.161615 10.25000 0.05407 AFIX 137 H6A1 2 0.273386 0.504930 0.177109 10.25000 -1.50000 H6A2 2 0.327011 0.549459 0.118433 10.25000 -1.50000 H6A3 2 0.410702 0.529678 0.208142 10.25000 -1.50000 AFIX 0 C7A 1 0.253446 0.415204 0.058212 10.25000 0.06251 AFIX 137 H7A1 2 0.190406 0.402042 0.079821 10.25000 -1.50000 H7A2 2 0.270945 0.371554 0.030116 10.25000 -1.50000 H7A3 2 0.226832 0.457375 0.020546 10.25000 -1.50000 AFIX 0 C8A 1 0.469593 0.445693 0.099025 10.25000 0.04732 AFIX 137 H8A1 2 0.455463 0.489890 0.063773 10.25000 -1.50000 H8A2 2 0.469880 0.400117 0.067774 10.25000 -1.50000 H8A3 2 0.546868 0.450847 0.142118 10.25000 -1.50000 AFIX 0 PART 0 C9 1 0.620389 0.292192 0.225780 11.00000 0.03387 0.04900 = 0.07964 0.02370 0.03347 0.01732 AFIX 137 H9A 2 0.578297 0.245704 0.202517 11.00000 -1.50000 H9B 2 0.696039 0.279524 0.267805 11.00000 -1.50000 H9C 2 0.636298 0.321680 0.183680 11.00000 -1.50000 AFIX 0 C10 1 0.626744 0.417247 0.340380 11.00000 0.02996 0.05240 = 0.09899 -0.00937 0.00702 -0.00765 AFIX 137 H10A 2 0.670039 0.446258 0.311953 11.00000 -1.50000 H10B 2 0.683863 0.390086 0.385356 11.00000 -1.50000 H10C 2 0.579406 0.451608 0.360885 11.00000 -1.50000 AFIX 0 C11 1 0.232899 0.533521 0.364873 11.00000 0.05962 0.04137 = 0.04502 -0.01906 0.00266 0.01105 PART 1 C12 1 0.255980 0.614573 0.329746 10.50000 0.05631 AFIX 137 H12A 2 0.310173 0.644744 0.373375 10.50000 -1.50000 H12B 2 0.179922 0.641242 0.306654 10.50000 -1.50000 H12C 2 0.291754 0.606577 0.288039 10.50000 -1.50000 AFIX 0 C13 1 0.186406 0.549580 0.428927 10.50000 0.07310 AFIX 137 H13A 2 0.140336 0.506223 0.436478 10.50000 -1.50000 H13B 2 0.134656 0.594064 0.414789 10.50000 -1.50000 H13C 2 0.252782 0.559314 0.478834 10.50000 -1.50000 AFIX 0 C14 1 0.338994 0.490940 0.401361 10.50000 0.06052 AFIX 137 H14A 2 0.318945 0.443451 0.422083 10.50000 -1.50000 H14B 2 0.393983 0.519954 0.445711 10.50000 -1.50000 H14C 2 0.377015 0.480132 0.361382 10.50000 -1.50000 AFIX 0 PART 2 C12A 1 0.221128 0.613363 0.356087 10.50000 0.07592 AFIX 137 H12D 2 0.166137 0.625543 0.302202 10.50000 -1.50000 H12E 2 0.299378 0.635731 0.363587 10.50000 -1.50000 H12F 2 0.189783 0.633679 0.396436 10.50000 -1.50000 AFIX 0 C13A 1 0.195471 0.511608 0.444536 10.50000 0.09515 AFIX 137 H13D 2 0.129336 0.543821 0.445837 10.50000 -1.50000 H13E 2 0.264216 0.519445 0.493590 10.50000 -1.50000 H13F 2 0.170801 0.458642 0.441136 10.50000 -1.50000 AFIX 0 C14A 1 0.360059 0.502284 0.379156 10.50000 0.04176 AFIX 137 H14D 2 0.362111 0.448358 0.391647 10.50000 -1.50000 H14E 2 0.417566 0.529112 0.424224 10.50000 -1.50000 H14F 2 0.380826 0.509648 0.330620 10.50000 -1.50000 AFIX 0 PART 0 C15 1 -0.094749 0.384719 0.127357 11.00000 0.02082 0.03308 = 0.03755 0.00289 0.00957 0.00423 C16 1 -0.215668 0.423858 0.110856 11.00000 0.01785 0.05467 = 0.05988 0.00696 0.00552 0.00413 AFIX 137 H16A 2 -0.239036 0.420618 0.158777 11.00000 -1.50000 H16B 2 -0.276074 0.398991 0.065682 11.00000 -1.50000 H16C 2 -0.209071 0.476947 0.097577 11.00000 -1.50000 AFIX 0 C17 1 -0.059256 0.389696 0.052411 11.00000 0.04332 0.04820 = 0.02873 -0.00013 0.00639 0.00219 AFIX 137 H17A 2 -0.051347 0.442763 0.039614 11.00000 -1.50000 H17B 2 -0.120735 0.365641 0.007192 11.00000 -1.50000 H17C 2 0.017117 0.363882 0.062276 11.00000 -1.50000 AFIX 0 C18 1 -0.106345 0.301921 0.147797 11.00000 0.03324 0.03308 = 0.05234 0.00092 0.01405 -0.00578 AFIX 137 H18A 2 -0.029835 0.276305 0.157578 11.00000 -1.50000 H18B 2 -0.167847 0.277590 0.102808 11.00000 -1.50000 H18C 2 -0.128783 0.298825 0.196100 11.00000 -1.50000 AFIX 0 C19 1 -0.105041 0.548930 0.271538 11.00000 0.06396 0.05341 = 0.07391 0.00040 0.03787 0.03131 AFIX 137 H19A 2 -0.114635 0.510882 0.309043 11.00000 -1.50000 H19B 2 -0.181427 0.556505 0.228183 11.00000 -1.50000 H19C 2 -0.078963 0.596586 0.300162 11.00000 -1.50000 AFIX 0 C20 1 0.011122 0.587792 0.150884 11.00000 0.06082 0.03152 = 0.06701 0.01514 0.02097 0.01409 AFIX 137 H20A 2 0.021833 0.638180 0.175037 11.00000 -1.50000 H20B 2 -0.064588 0.585870 0.105905 11.00000 -1.50000 H20C 2 0.077057 0.576867 0.131289 11.00000 -1.50000 AFIX 0 C23 1 -0.018276 0.352242 0.381267 11.00000 0.04890 0.06401 = 0.05492 0.02320 0.03542 0.02453 AFIX 23 H23A 2 0.003270 0.402145 0.407234 11.00000 -1.20000 H23B 2 -0.084495 0.359438 0.329785 11.00000 -1.20000 AFIX 0 C24 1 -0.057459 0.301405 0.434377 11.00000 0.05039 0.08907 = 0.06556 0.02961 0.03589 0.01888 AFIX 137 H24A 2 -0.082842 0.252972 0.407294 11.00000 -1.50000 H24B 2 -0.124325 0.324560 0.446182 11.00000 -1.50000 H24C 2 0.008972 0.293190 0.484647 11.00000 -1.50000 AFIX 0 PART 1 C21A 1 0.329080 0.195835 0.131873 10.50000 0.05152 AFIX 23 H21A 2 0.358970 0.227342 0.096589 10.50000 -1.20000 H21B 2 0.393695 0.190677 0.184466 10.50000 -1.20000 AFIX 0 C22A 1 0.294821 0.120843 0.095443 10.50000 0.05879 AFIX 137 H22A 2 0.217045 0.124144 0.052541 10.50000 -1.50000 H22B 2 0.289803 0.085300 0.136582 10.50000 -1.50000 H22C 2 0.354836 0.103220 0.072982 10.50000 -1.50000 AFIX 0 PART 2 C21 1 0.299976 0.207728 0.100571 10.50000 0.02652 AFIX 23 H21C 2 0.259088 0.202935 0.041848 10.50000 -1.20000 H21D 2 0.365387 0.244782 0.109666 10.50000 -1.20000 AFIX 0 C22 1 0.352742 0.131415 0.134682 10.50000 0.04962 AFIX 137 H22D 2 0.410048 0.115353 0.109190 10.50000 -1.50000 H22E 2 0.288623 0.094046 0.123921 10.50000 -1.50000 H22F 2 0.393409 0.135885 0.192818 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 REM pst_014s P 21 R = New: P21/c REM R1 = 0.0594 for 10491 Fo > 4sig(Fo) and 0.0862 for all 13009 data REM 325 parameters refined using 0 restraints END WGHT 0.0000 12.9243 REM Highest difference peak 0.779, deepest hole -1.009, 1-sigma level 0.105 Q1 1 0.4779 0.4786 0.1244 11.00000 0.05 0.78 Q2 1 0.4121 0.4040 0.0712 11.00000 0.05 0.74 Q3 1 0.3058 0.3950 0.0458 11.00000 0.05 0.74 Q4 1 0.3744 0.4079 0.3091 11.00000 0.05 0.70 Q5 1 0.4494 0.2699 0.1970 11.00000 0.05 0.69 Q6 1 0.1078 0.3586 0.2731 11.00000 0.05 0.69 Q7 1 0.2658 0.2554 0.3211 11.00000 0.05 0.68 Q8 1 0.3338 0.3578 0.2221 11.00000 0.05 0.66 Q9 1 0.4217 0.2015 0.2754 11.00000 0.05 0.64 Q10 1 0.4516 0.3898 0.1992 11.00000 0.05 0.64 ; _shelx_res_checksum 7790 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Ge1 Ge 0.29426(4) 0.32966(2) 0.23351(3) 0.02044(8) Uani 1 1 d . . . . . Ge2 Ge 0.13528(4) 0.39147(2) 0.27161(3) 0.02286(9) Uani 1 1 d . . . . . Si1 Si 0.52622(11) 0.34867(7) 0.27021(10) 0.0330(3) Uani 1 1 d . . . . . Si2 Si 0.00933(13) 0.51612(7) 0.22805(9) 0.0335(3) Uani 1 1 d . . . . . S1 S 0.19549(11) 0.24210(7) 0.14589(8) 0.0361(3) Uani 1 1 d . . . . . S2 S 0.11054(12) 0.31169(8) 0.36202(8) 0.0384(3) Uani 1 1 d . . . . . N1 N 0.4354(3) 0.2956(2) 0.3086(2) 0.0255(7) Uani 1 1 d . . . . . N2 N 0.3985(3) 0.3866(2) 0.2002(3) 0.0310(8) Uani 1 1 d . . . . . N3 N 0.1477(4) 0.4926(2) 0.2984(2) 0.0329(8) Uani 1 1 d . . . . . N4 N -0.0063(3) 0.4227(2) 0.1958(2) 0.0247(7) Uani 1 1 d . . . . . C1 C 0.4617(4) 0.2457(3) 0.3781(3) 0.0328(9) Uani 1 1 d . . . . . C2 C 0.4627(6) 0.2894(4) 0.4527(3) 0.0506(14) Uani 1 1 d . . . . . H2A H 0.5231 0.3292 0.4641 0.076 Uiso 1 1 calc R U . . . H2B H 0.4815 0.2549 0.4986 0.076 Uiso 1 1 calc R U . . . H2C H 0.3840 0.3120 0.4432 0.076 Uiso 1 1 calc R U . . . C3 C 0.3659(5) 0.1838(3) 0.3615(3) 0.0401(11) Uani 1 1 d . . . . . H3A H 0.2871 0.2071 0.3491 0.060 Uiso 1 1 calc R U . . . H3B H 0.3823 0.1516 0.4091 0.060 Uiso 1 1 calc R U . . . H3C H 0.3673 0.1531 0.3158 0.060 Uiso 1 1 calc R U . . . C4 C 0.5840(5) 0.2087(4) 0.3941(4) 0.0556(16) Uani 1 1 d . . . . . H4A H 0.5836 0.1802 0.3466 0.083 Uiso 1 1 calc R U . . . H4B H 0.6010 0.1744 0.4401 0.083 Uiso 1 1 calc R U . . . H4C H 0.6457 0.2478 0.4060 0.083 Uiso 1 1 calc R U . . . C5 C 0.3764(5) 0.4401(3) 0.1334(3) 0.0365(11) Uani 1 1 d . . . . . C6 C 0.4870(8) 0.4950(5) 0.1561(6) 0.057(2) Uiso 0.75 1 d . . P A 1 H6A H 0.4817 0.5270 0.1099 0.086 Uiso 0.75 1 calc R U P A 1 H6B H 0.5607 0.4653 0.1710 0.086 Uiso 0.75 1 calc R U P A 1 H6C H 0.4874 0.5267 0.2016 0.086 Uiso 0.75 1 calc R U P A 1 C7 C 0.2710(7) 0.4871(4) 0.1246(5) 0.0415(15) Uiso 0.75 1 d . . P A 1 H7A H 0.2650 0.5267 0.0848 0.062 Uiso 0.75 1 calc R U P A 1 H7B H 0.2787 0.5102 0.1764 0.062 Uiso 0.75 1 calc R U P A 1 H7C H 0.1992 0.4556 0.1068 0.062 Uiso 0.75 1 calc R U P A 1 C8 C 0.3714(10) 0.3996(6) 0.0601(6) 0.066(3) Uiso 0.75 1 d . . P A 1 H8A H 0.4445 0.3700 0.0703 0.100 Uiso 0.75 1 calc R U P A 1 H8B H 0.3641 0.4359 0.0169 0.100 Uiso 0.75 1 calc R U P A 1 H8C H 0.3022 0.3657 0.0440 0.100 Uiso 0.75 1 calc R U P A 1 C6A C 0.344(3) 0.5120(15) 0.1616(17) 0.054(6) Uiso 0.25 1 d . . P A 2 H6A1 H 0.2734 0.5049 0.1771 0.081 Uiso 0.25 1 calc R U P A 2 H6A2 H 0.3270 0.5495 0.1184 0.081 Uiso 0.25 1 calc R U P A 2 H6A3 H 0.4107 0.5297 0.2081 0.081 Uiso 0.25 1 calc R U P A 2 C7A C 0.253(3) 0.4152(18) 0.0582(18) 0.063(7) Uiso 0.25 1 d . . P A 2 H7A1 H 0.1904 0.4020 0.0798 0.094 Uiso 0.25 1 calc R U P A 2 H7A2 H 0.2709 0.3716 0.0301 0.094 Uiso 0.25 1 calc R U P A 2 H7A3 H 0.2268 0.4574 0.0205 0.094 Uiso 0.25 1 calc R U P A 2 C8A C 0.470(2) 0.4457(14) 0.0990(15) 0.047(5) Uiso 0.25 1 d . . P A 2 H8A1 H 0.4555 0.4899 0.0638 0.071 Uiso 0.25 1 calc R U P A 2 H8A2 H 0.4699 0.4001 0.0678 0.071 Uiso 0.25 1 calc R U P A 2 H8A3 H 0.5469 0.4508 0.1421 0.071 Uiso 0.25 1 calc R U P A 2 C9 C 0.6204(5) 0.2922(3) 0.2258(4) 0.0505(15) Uani 1 1 d . . . . . H9A H 0.5783 0.2457 0.2025 0.076 Uiso 1 1 calc R U . . . H9B H 0.6960 0.2795 0.2678 0.076 Uiso 1 1 calc R U . . . H9C H 0.6363 0.3217 0.1837 0.076 Uiso 1 1 calc R U . . . C10 C 0.6267(5) 0.4172(4) 0.3404(5) 0.064(2) Uani 1 1 d . . . . . H10A H 0.6700 0.4463 0.3120 0.096 Uiso 1 1 calc R U . . . H10B H 0.6839 0.3901 0.3854 0.096 Uiso 1 1 calc R U . . . H10C H 0.5794 0.4516 0.3609 0.096 Uiso 1 1 calc R U . . . C11 C 0.2329(6) 0.5335(3) 0.3649(4) 0.0525(16) Uani 1 1 d . . . . . C12 C 0.2560(14) 0.6146(8) 0.3297(9) 0.056(3) Uiso 0.5 1 d . . P B 1 H12A H 0.3102 0.6447 0.3734 0.084 Uiso 0.5 1 calc R U P B 1 H12B H 0.1799 0.6412 0.3067 0.084 Uiso 0.5 1 calc R U P B 1 H12C H 0.2918 0.6066 0.2880 0.084 Uiso 0.5 1 calc R U P B 1 C13 C 0.1864(17) 0.5496(11) 0.4289(11) 0.073(5) Uiso 0.5 1 d . . P B 1 H13A H 0.1403 0.5062 0.4365 0.110 Uiso 0.5 1 calc R U P B 1 H13B H 0.1347 0.5941 0.4148 0.110 Uiso 0.5 1 calc R U P B 1 H13C H 0.2528 0.5593 0.4788 0.110 Uiso 0.5 1 calc R U P B 1 C14 C 0.3390(15) 0.4909(9) 0.4014(10) 0.061(4) Uiso 0.5 1 d . . P B 1 H14A H 0.3189 0.4435 0.4221 0.091 Uiso 0.5 1 calc R U P B 1 H14B H 0.3940 0.5200 0.4457 0.091 Uiso 0.5 1 calc R U P B 1 H14C H 0.3770 0.4801 0.3614 0.091 Uiso 0.5 1 calc R U P B 1 C12A C 0.2211(17) 0.6134(10) 0.3561(12) 0.076(5) Uiso 0.5 1 d . . P B 2 H12D H 0.1661 0.6255 0.3022 0.114 Uiso 0.5 1 calc R U P B 2 H12E H 0.2994 0.6357 0.3636 0.114 Uiso 0.5 1 calc R U P B 2 H12F H 0.1898 0.6337 0.3964 0.114 Uiso 0.5 1 calc R U P B 2 C13A C 0.195(2) 0.5116(14) 0.4445(13) 0.095(7) Uiso 0.5 1 d . . P B 2 H13D H 0.1293 0.5438 0.4458 0.143 Uiso 0.5 1 calc R U P B 2 H13E H 0.2642 0.5194 0.4936 0.143 Uiso 0.5 1 calc R U P B 2 H13F H 0.1708 0.4586 0.4411 0.143 Uiso 0.5 1 calc R U P B 2 C14A C 0.3601(11) 0.5023(7) 0.3792(8) 0.042(2) Uiso 0.5 1 d . . P B 2 H14D H 0.3621 0.4484 0.3916 0.063 Uiso 0.5 1 calc R U P B 2 H14E H 0.4176 0.5291 0.4242 0.063 Uiso 0.5 1 calc R U P B 2 H14F H 0.3808 0.5096 0.3306 0.063 Uiso 0.5 1 calc R U P B 2 C15 C -0.0947(4) 0.3847(3) 0.1274(3) 0.0306(9) Uani 1 1 d . . . . . C16 C -0.2157(4) 0.4239(4) 0.1109(4) 0.0461(13) Uani 1 1 d . . . . . H16A H -0.2390 0.4206 0.1588 0.069 Uiso 1 1 calc R U . . . H16B H -0.2761 0.3990 0.0657 0.069 Uiso 1 1 calc R U . . . H16C H -0.2091 0.4769 0.0976 0.069 Uiso 1 1 calc R U . . . C17 C -0.0593(5) 0.3897(3) 0.0524(3) 0.0416(11) Uani 1 1 d . . . . . H17A H -0.0513 0.4428 0.0396 0.062 Uiso 1 1 calc R U . . . H17B H -0.1207 0.3656 0.0072 0.062 Uiso 1 1 calc R U . . . H17C H 0.0171 0.3639 0.0623 0.062 Uiso 1 1 calc R U . . . C18 C -0.1063(5) 0.3019(3) 0.1478(4) 0.0397(11) Uani 1 1 d . . . . . H18A H -0.0298 0.2763 0.1576 0.060 Uiso 1 1 calc R U . . . H18B H -0.1678 0.2776 0.1028 0.060 Uiso 1 1 calc R U . . . H18C H -0.1288 0.2988 0.1961 0.060 Uiso 1 1 calc R U . . . C19 C -0.1050(6) 0.5489(4) 0.2715(5) 0.0601(18) Uani 1 1 d . . . . . H19A H -0.1146 0.5109 0.3090 0.090 Uiso 1 1 calc R U . . . H19B H -0.1814 0.5565 0.2282 0.090 Uiso 1 1 calc R U . . . H19C H -0.0790 0.5966 0.3002 0.090 Uiso 1 1 calc R U . . . C20 C 0.0111(6) 0.5878(3) 0.1509(4) 0.0533(15) Uani 1 1 d . . . . . H20A H 0.0218 0.6382 0.1750 0.080 Uiso 1 1 calc R U . . . H20B H -0.0646 0.5859 0.1059 0.080 Uiso 1 1 calc R U . . . H20C H 0.0771 0.5769 0.1313 0.080 Uiso 1 1 calc R U . . . C23 C -0.0183(6) 0.3522(4) 0.3813(4) 0.0514(16) Uani 1 1 d . . . . . H23A H 0.0033 0.4021 0.4072 0.062 Uiso 1 1 calc R U . . . H23B H -0.0845 0.3594 0.3298 0.062 Uiso 1 1 calc R U . . . C24 C -0.0575(6) 0.3014(5) 0.4344(4) 0.064(2) Uani 1 1 d . . . . . H24A H -0.0828 0.2530 0.4073 0.096 Uiso 1 1 calc R U . . . H24B H -0.1243 0.3246 0.4462 0.096 Uiso 1 1 calc R U . . . H24C H 0.0090 0.2932 0.4846 0.096 Uiso 1 1 calc R U . . . C21A C 0.3291(13) 0.1958(8) 0.1319(9) 0.052(3) Uiso 0.5 1 d . . P C 1 H21A H 0.3590 0.2273 0.0966 0.062 Uiso 0.5 1 calc R U P C 1 H21B H 0.3937 0.1907 0.1845 0.062 Uiso 0.5 1 calc R U P C 1 C22A C 0.2948(14) 0.1208(8) 0.0954(9) 0.059(3) Uiso 0.5 1 d . . P C 1 H22A H 0.2170 0.1241 0.0525 0.088 Uiso 0.5 1 calc R U P C 1 H22B H 0.2898 0.0853 0.1366 0.088 Uiso 0.5 1 calc R U P C 1 H22C H 0.3548 0.1032 0.0730 0.088 Uiso 0.5 1 calc R U P C 1 C21 C 0.3000(9) 0.2077(5) 0.1006(6) 0.0265(16) Uiso 0.5 1 d . . P C 2 H21C H 0.2591 0.2029 0.0418 0.032 Uiso 0.5 1 calc R U P C 2 H21D H 0.3654 0.2448 0.1097 0.032 Uiso 0.5 1 calc R U P C 2 C22 C 0.3527(12) 0.1314(7) 0.1347(8) 0.050(3) Uiso 0.5 1 d . . P C 2 H22D H 0.4100 0.1154 0.1092 0.074 Uiso 0.5 1 calc R U P C 2 H22E H 0.2886 0.0940 0.1239 0.074 Uiso 0.5 1 calc R U P C 2 H22F H 0.3934 0.1359 0.1928 0.074 Uiso 0.5 1 calc R U P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01990(17) 0.01826(16) 0.02499(19) 0.00127(16) 0.01004(16) 0.00220(14) Ge2 0.02424(19) 0.02109(17) 0.0257(2) 0.00141(16) 0.01172(17) 0.00504(15) Si1 0.0218(5) 0.0264(5) 0.0518(8) 0.0039(6) 0.0137(6) 0.0021(4) Si2 0.0373(7) 0.0243(5) 0.0426(7) 0.0036(5) 0.0185(6) 0.0120(5) S1 0.0326(6) 0.0320(5) 0.0424(7) -0.0130(5) 0.0111(5) 0.0010(4) S2 0.0393(6) 0.0431(6) 0.0414(7) 0.0188(5) 0.0250(6) 0.0177(5) N1 0.0193(15) 0.0268(16) 0.0280(18) 0.0041(14) 0.0047(13) 0.0049(12) N2 0.0284(17) 0.0264(16) 0.042(2) 0.0133(16) 0.0174(16) 0.0068(14) N3 0.040(2) 0.0250(16) 0.0333(19) -0.0061(15) 0.0122(17) 0.0094(16) N4 0.0218(15) 0.0227(15) 0.0303(18) 0.0033(13) 0.0097(14) 0.0058(12) C1 0.031(2) 0.034(2) 0.032(2) 0.0046(18) 0.0086(18) 0.0084(18) C2 0.064(4) 0.055(3) 0.030(3) 0.003(2) 0.012(3) 0.009(3) C3 0.050(3) 0.033(2) 0.043(3) 0.014(2) 0.023(2) 0.006(2) C4 0.039(3) 0.058(4) 0.063(4) 0.024(3) 0.009(3) 0.023(3) C5 0.045(3) 0.0254(19) 0.050(3) 0.012(2) 0.030(2) 0.0038(19) C9 0.034(3) 0.049(3) 0.080(4) 0.024(3) 0.033(3) 0.017(2) C10 0.030(3) 0.052(4) 0.099(6) -0.009(4) 0.007(3) -0.008(3) C11 0.060(4) 0.041(3) 0.045(3) -0.019(3) 0.003(3) 0.011(3) C15 0.0208(18) 0.033(2) 0.038(2) 0.0029(18) 0.0096(17) 0.0042(16) C16 0.018(2) 0.055(3) 0.060(4) 0.007(3) 0.006(2) 0.004(2) C17 0.043(3) 0.048(3) 0.029(2) 0.000(2) 0.006(2) 0.002(2) C18 0.033(2) 0.033(2) 0.052(3) 0.001(2) 0.014(2) -0.006(2) C19 0.064(4) 0.053(3) 0.074(4) 0.000(3) 0.038(4) 0.031(3) C20 0.061(4) 0.032(2) 0.067(4) 0.015(3) 0.021(3) 0.014(2) C23 0.049(3) 0.064(4) 0.055(4) 0.023(3) 0.035(3) 0.025(3) C24 0.050(4) 0.089(5) 0.066(4) 0.030(4) 0.036(3) 0.019(4) 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' Ge Ge 0.1547 1.8001 '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 N2 Ge1 N1 82.05(16) N2 Ge1 S1 114.39(14) N1 Ge1 S1 114.03(12) N2 Ge1 Ge2 120.39(12) N1 Ge1 Ge2 122.81(12) S1 Ge1 Ge2 103.08(4) N2 Ge1 Si1 41.04(12) N1 Ge1 Si1 41.05(12) S1 Ge1 Si1 121.48(5) Ge2 Ge1 Si1 135.42(4) N3 Ge2 N4 82.47(17) N3 Ge2 S2 116.80(13) N4 Ge2 S2 113.60(12) N3 Ge2 Ge1 119.85(14) N4 Ge2 Ge1 122.02(11) S2 Ge2 Ge1 102.41(4) N3 Ge2 Si2 41.33(14) N4 Ge2 Si2 41.20(12) S2 Ge2 Si2 122.76(5) Ge1 Ge2 Si2 134.83(4) N1 Si1 N2 88.69(17) N1 Si1 C10 116.1(3) N2 Si1 C10 115.7(3) N1 Si1 C9 114.7(2) N2 Si1 C9 114.5(3) C10 Si1 C9 106.8(3) N1 Si1 Ge1 44.53(12) N2 Si1 Ge1 44.21(12) C10 Si1 Ge1 129.2(2) C9 Si1 Ge1 123.9(2) N4 Si2 N3 88.59(18) N4 Si2 C20 115.7(3) N3 Si2 C20 116.1(3) N4 Si2 C19 114.8(3) N3 Si2 C19 115.2(3) C20 Si2 C19 106.2(3) N4 Si2 Ge2 44.33(12) N3 Si2 Ge2 44.33(13) C20 Si2 Ge2 129.5(2) C19 Si2 Ge2 124.2(2) C21 S1 Ge1 105.3(3) C21A S1 Ge1 97.2(4) C23 S2 Ge2 102.02(19) C1 N1 Si1 132.4(3) C1 N1 Ge1 133.1(3) Si1 N1 Ge1 94.43(18) C5 N2 Si1 134.2(3) C5 N2 Ge1 130.9(3) Si1 N2 Ge1 94.75(18) C11 N3 Si2 133.2(3) C11 N3 Ge2 131.5(3) Si2 N3 Ge2 94.3(2) C15 N4 Si2 132.2(3) C15 N4 Ge2 133.0(3) Si2 N4 Ge2 94.48(18) N1 C1 C2 110.9(4) N1 C1 C4 109.5(4) C2 C1 C4 109.2(5) N1 C1 C3 109.8(4) C2 C1 C3 108.3(5) C4 C1 C3 109.1(4) C8A C5 C6A 114.4(16) C8A C5 N2 115.5(11) C6A C5 N2 106.5(11) C8 C5 N2 109.7(5) C8 C5 C7 114.0(7) N2 C5 C7 111.4(5) C8 C5 C6 107.9(6) N2 C5 C6 106.8(5) C7 C5 C6 106.7(5) C8A C5 C7A 106.0(15) C6A C5 C7A 104.0(16) N2 C5 C7A 109.8(11) C14 C11 C13 105.4(11) C14 C11 N3 111.6(8) C12A C11 N3 113.0(9) C13 C11 N3 112.5(9) C12A C11 C14A 115.3(10) N3 C11 C14A 109.1(6) C14 C11 C12 113.7(10) C13 C11 C12 106.5(10) N3 C11 C12 107.1(7) C12A C11 C13A 106.2(12) N3 C11 C13A 104.7(10) C14A C11 C13A 107.9(10) N4 C15 C17 110.9(4) N4 C15 C18 110.0(4) C17 C15 C18 109.6(4) N4 C15 C16 108.2(4) C17 C15 C16 109.2(4) C18 C15 C16 108.9(4) C24 C23 S2 110.1(4) C22A C21A S1 109.3(10) C22 C21 S1 112.2(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ge1 N2 1.845(4) Ge1 N1 1.855(3) Ge1 S1 2.2271(13) Ge1 Ge2 2.4727(6) Ge1 Si1 2.6374(13) Ge2 N3 1.847(4) Ge2 N4 1.847(4) Ge2 S2 2.2290(12) Ge2 Si2 2.6358(13) Si1 N1 1.737(4) Si1 N2 1.738(4) Si1 C10 1.856(7) Si1 C9 1.866(6) Si2 N4 1.741(4) Si2 N3 1.746(4) Si2 C20 1.871(6) Si2 C19 1.871(6) S1 C21 1.801(9) S1 C21A 1.881(14) S2 C23 1.829(5) N1 C1 1.460(6) N2 C5 1.469(6) N3 C11 1.460(7) N4 C15 1.471(6) C1 C2 1.527(7) C1 C4 1.535(7) C1 C3 1.539(7) C5 C8A 1.44(2) C5 C6A 1.47(3) C5 C8 1.468(11) C5 C7 1.470(9) C5 C6 1.577(11) C5 C7A 1.67(3) C11 C14 1.425(17) C11 C12A 1.426(19) C11 C13 1.449(19) C11 C14A 1.551(14) C11 C12 1.626(16) C11 C13A 1.66(2) C15 C17 1.525(7) C15 C18 1.530(7) C15 C16 1.535(6) C23 C24 1.487(8) C21A C22A 1.47(2) C21 C22 1.528(16)