#------------------------------------------------------------------------------ #$Date: 2016-04-08 03:44:04 +0300 (Fri, 08 Apr 2016) $ #$Revision: 181968 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/64/4086454.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_4086454 loop_ _publ_author_name 'Seow, Celestine' 'Xi, Hong-Wei' 'Li, Yongxin' 'So, Cheuk-Wai' _publ_section_title ; Synthesis of a Germylidenide Anion from the C--C Bond Activation of a Bis(germylene) ; _journal_name_full Organometallics _journal_paper_doi 10.1021/acs.organomet.5b01001 _journal_year 2016 _chemical_formula_sum 'C16 H23 Cl Ge N2' _chemical_formula_weight 351.40 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _cell_angle_alpha 90 _cell_angle_beta 95.918(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7947(6) _cell_length_b 16.4126(11) _cell_length_c 11.7594(8) _cell_measurement_reflns_used 9960 _cell_measurement_temperature 103.(2) _cell_measurement_theta_max 32.3905 _cell_measurement_theta_min 2.4819 _cell_volume 1688.4(2) _computing_cell_refinement 'SAINT V8.35A (Bruker AXS Inc., 2015)' _computing_data_collection 'APEX3 (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.35A (Bruker AXS Inc., 2015)' _computing_molecular_graphics 'XP (Bruker AXS Inc., 2015)' _computing_publication_material 'APEX3 (Bruker AXS Inc., 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'XT, VERSION 2014/4' _diffrn_ambient_temperature 103.(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_unetI/netI 0.0461 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 29237 _diffrn_reflns_theta_full 32.51 _diffrn_reflns_theta_max 32.51 _diffrn_reflns_theta_min 2.14 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker KappaCCD' _exptl_absorpt_coefficient_mu 1.965 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.180 _refine_diff_density_max 1.104 _refine_diff_density_min -0.774 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 5968 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0377 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+1.4925P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.0946 _reflns_number_gt 4590 _reflns_number_total 5968 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file om5b01001_si_002.cif _cod_data_source_block scw1387s _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-Scan' changed to 'multi-scan' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas ; _cod_database_code 4086454 _shelx_res_file ; scw1387s.res created by SHELXL-2014/7 TITL scw1387s in P2(1)/n CELL 0.71073 8.79470 16.41260 11.75940 90.0000 95.9176 90.0000 ZERR 4.00 0.00060 0.00110 0.00080 0.0000 0.0022 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N Cl Ge UNIT 64 92 8 4 4 L.S. 14 ACTA BOND FMAP 2 PLAN 5 SIZE 0.18 0.22 0.42 TEMP -170 WGHT 0.039500 1.492500 FVAR 0.14253 GE1 5 0.761881 0.863202 0.940526 11.00000 0.00892 0.01544 = 0.01725 -0.00292 0.00021 0.00030 CL1 4 0.799923 0.730293 0.875307 11.00000 0.01405 0.01411 = 0.01516 -0.00676 -0.00082 -0.00023 C1 1 0.984769 0.890438 0.957404 11.00000 0.01205 0.01113 = 0.01370 -0.00255 0.00093 0.00053 C2 1 1.057554 0.928698 0.871837 11.00000 0.01274 0.01166 = 0.01432 -0.00165 0.00167 0.00098 C3 1 1.213586 0.947259 0.889681 11.00000 0.01295 0.01436 = 0.02042 0.00040 0.00214 -0.00161 AFIX 43 H3 2 1.262258 0.973682 0.831341 11.00000 -1.20000 AFIX 0 C4 1 1.297772 0.927050 0.992924 11.00000 0.01156 0.01878 = 0.02090 -0.00210 -0.00069 -0.00332 AFIX 43 H4 2 1.403931 0.939032 1.004309 11.00000 -1.20000 AFIX 0 C5 1 1.226561 0.889393 1.079213 11.00000 0.01363 0.01799 = 0.01707 -0.00140 -0.00247 -0.00065 AFIX 43 H5 2 1.283393 0.875541 1.149666 11.00000 -1.20000 AFIX 0 C6 1 1.070004 0.872166 1.060874 11.00000 0.01248 0.01298 = 0.01382 -0.00167 0.00072 -0.00058 C7 1 0.985224 0.835194 1.148736 11.00000 0.01707 0.01515 = 0.01240 -0.00004 0.00012 0.00179 AFIX 43 H7 2 1.034346 0.822473 1.222351 11.00000 -1.20000 AFIX 0 C8 1 0.742820 0.788570 1.207068 11.00000 0.01805 0.01839 = 0.01523 0.00306 0.00461 -0.00269 C9 1 0.831877 0.754285 1.315407 11.00000 0.02797 0.02652 = 0.02084 0.00934 0.00681 0.00394 AFIX 137 H9A 2 0.898859 0.710167 1.294671 11.00000 -1.50000 H9B 2 0.759965 0.733127 1.366532 11.00000 -1.50000 H9C 2 0.893772 0.797630 1.354316 11.00000 -1.50000 AFIX 0 C10 1 0.643867 0.859987 1.239130 11.00000 0.01988 0.02839 = 0.02463 0.00831 0.00996 0.00472 AFIX 137 H10A 2 0.708310 0.900429 1.282321 11.00000 -1.50000 H10B 2 0.565913 0.840146 1.286180 11.00000 -1.50000 H10C 2 0.593997 0.885129 1.169425 11.00000 -1.50000 AFIX 0 C11 1 0.641321 0.723295 1.146305 11.00000 0.04225 0.03166 = 0.02490 0.00161 0.00712 -0.02009 AFIX 137 H11A 2 0.588003 0.746033 1.076127 11.00000 -1.50000 H11B 2 0.566210 0.704771 1.196680 11.00000 -1.50000 H11C 2 0.704496 0.677116 1.127043 11.00000 -1.50000 AFIX 0 C12 1 0.965426 0.945698 0.762411 11.00000 0.01587 0.01283 = 0.01361 0.00031 0.00322 0.00082 AFIX 43 H12 2 1.007789 0.975245 0.703768 11.00000 -1.20000 AFIX 0 C13 1 0.728152 0.931791 0.639911 11.00000 0.01509 0.02294 = 0.01345 0.00083 -0.00077 0.00121 C14 1 0.804478 0.976133 0.546719 11.00000 0.02739 0.04671 = 0.01876 0.01366 -0.00420 -0.00415 AFIX 137 H14A 2 0.835905 1.030683 0.573680 11.00000 -1.50000 H14B 2 0.732029 0.980805 0.477903 11.00000 -1.50000 H14C 2 0.894472 0.945363 0.528780 11.00000 -1.50000 AFIX 0 C15 1 0.678606 0.847322 0.598586 11.00000 0.03383 0.03327 = 0.02006 -0.00333 -0.00864 -0.00649 AFIX 137 H15A 2 0.768074 0.816495 0.579709 11.00000 -1.50000 H15B 2 0.605026 0.852034 0.530416 11.00000 -1.50000 H15C 2 0.630731 0.818904 0.658955 11.00000 -1.50000 AFIX 0 C16 1 0.590003 0.980423 0.670950 11.00000 0.02825 0.06160 = 0.02317 -0.00582 -0.00548 0.02417 AFIX 137 H16A 2 0.546173 0.953691 0.734578 11.00000 -1.50000 H16B 2 0.512998 0.982998 0.604591 11.00000 -1.50000 H16C 2 0.622295 1.035749 0.693575 11.00000 -1.50000 AFIX 0 N1 3 0.842714 0.820615 1.122946 11.00000 0.01378 0.01377 = 0.01312 0.00135 0.00211 -0.00044 N2 3 0.827774 0.920025 0.747856 11.00000 0.01447 0.01480 = 0.01274 -0.00093 0.00093 0.00226 HKLF 4 REM scw1387s in P2(1)/n REM R1 = 0.0377 for 4590 Fo > 4sig(Fo) and 0.0592 for all 5968 data REM 187 parameters refined using 0 restraints END WGHT 0.0395 1.4866 REM Highest difference peak 1.104, deepest hole -0.774, 1-sigma level 0.102 Q1 1 0.7913 0.7036 0.8881 11.00000 0.05 1.10 Q2 1 0.8383 0.7336 0.8914 11.00000 0.05 1.07 Q3 1 0.7545 0.7344 0.8572 11.00000 0.05 1.04 Q4 1 0.7901 0.7489 0.8953 11.00000 0.05 0.95 Q5 1 0.8642 0.8710 0.9240 11.00000 0.05 0.53 ; _shelx_res_checksum 58327 _shelx_hkl_file ; -1 0 0 0.79 0.12 1 0 0 0.90 0.12 1 0 0 0.60 0.11 1 0 0 0.46 0.10 -1 0 0 0.71 0.10 -1 0 0 0.34 0.12 2 0 0 950.73 31.46 -2 0 0 973.83 31.38 -2 0 0 939.72 31.23 -2 0 0 987.11 31.17 2 0 0 1000.00 31.19 -2 0 0 953.06 31.32 2 0 0 933.18 31.53 -3 0 0 -0.16 0.22 3 0 0 0.02 0.22 -3 0 0 0.46 0.26 -3 0 0 0.06 0.22 3 0 0 0.01 0.19 3 0 0 -0.44 0.24 -3 0 0 0.31 0.09 4 0 0 339.08 11.38 -4 0 0 353.15 11.18 -4 0 0 342.87 11.44 -4 0 0 336.75 11.43 -5 0 0 0.21 0.47 5 0 0 -0.05 0.35 -6 0 0 32.42 1.66 6 0 0 35.14 1.61 7 0 0 -0.20 0.47 -7 0 0 -0.25 0.65 8 0 0 8.48 0.97 -8 0 0 10.20 1.25 -9 0 0 0.11 0.93 9 0 0 0.16 0.59 10 0 0 8.48 1.14 -10 0 0 7.93 1.26 -11 0 0 -0.18 0.90 -12 0 0 7.35 1.50 1 -1 0 90.76 3.05 1 -1 0 92.03 3.04 1 -1 0 89.61 3.03 -1 -1 0 89.77 3.04 -1 -1 0 94.36 2.99 -1 -1 0 93.23 3.07 -1 -1 0 88.77 3.00 -1 1 0 92.49 3.03 1 1 0 90.78 3.07 -1 1 0 90.74 3.05 1 1 0 91.22 3.00 -1 1 0 90.24 3.04 2 -1 0 16.09 0.66 -2 -1 0 16.75 0.70 -2 -1 0 17.74 0.77 2 -1 0 16.60 0.76 2 -1 0 18.93 0.75 -2 -1 0 16.60 0.76 2 1 0 16.75 0.76 2 1 0 16.57 0.76 -2 1 0 18.08 0.75 -2 1 0 16.45 0.67 -2 1 0 17.13 0.74 2 1 0 15.85 0.68 -3 -1 0 3.79 0.16 3 -1 0 3.91 0.39 3 -1 0 3.34 0.27 -3 -1 0 2.87 0.36 -3 -1 0 4.01 0.49 -3 -1 0 3.33 0.37 3 -1 0 3.21 0.37 3 1 0 3.55 0.44 3 1 0 3.46 0.40 -3 1 0 4.01 0.42 -3 1 0 3.40 0.39 3 1 0 3.39 0.36 -3 1 0 4.70 0.45 -3 1 0 4.25 0.30 -4 -1 0 124.15 4.40 4 -1 0 124.46 4.45 -4 -1 0 124.30 4.47 4 -1 0 129.30 4.23 4 1 0 123.49 4.50 -4 1 0 133.92 4.24 4 1 0 124.72 4.37 -4 1 0 126.59 4.47 -4 1 0 129.11 4.45 5 -1 0 44.75 1.92 5 -1 0 46.31 1.60 -5 -1 0 44.42 1.92 5 1 0 45.59 1.96 -5 1 0 46.11 1.60 5 1 0 41.90 1.82 -5 1 0 43.53 1.97 6 -1 0 67.68 2.61 -6 -1 0 60.60 2.65 -6 1 0 58.85 2.64 6 1 0 63.15 2.48 -7 -1 0 6.64 0.97 7 -1 0 7.33 0.91 -7 1 0 5.99 0.83 7 1 0 5.93 0.73 -8 -1 0 12.29 1.18 8 -1 0 8.78 1.16 8 1 0 10.92 1.03 -8 1 0 8.62 1.21 -9 -1 0 4.83 0.96 9 -1 0 2.61 0.79 -9 1 0 3.78 0.90 9 1 0 3.68 0.76 10 -1 0 10.26 1.20 -10 -1 0 9.25 1.34 10 1 0 8.55 1.02 -10 1 0 10.56 1.58 -11 -1 0 7.83 1.36 -11 1 0 10.67 1.53 -12 -1 0 0.23 1.03 -12 1 0 0.94 1.40 0 -2 0 40.94 1.53 0 -2 0 43.77 1.46 0 -2 0 43.51 1.46 0 2 0 42.75 1.53 0 2 0 42.88 1.46 0 2 0 43.56 1.46 1 -2 0 411.41 13.10 -1 -2 0 389.42 13.08 1 -2 0 402.26 13.13 -1 -2 0 397.58 13.16 1 -2 0 403.71 13.11 -1 -2 0 406.14 13.15 -1 2 0 422.72 13.12 1 2 0 402.64 13.21 1 2 0 386.08 13.15 1 2 0 387.79 13.14 -1 2 0 410.02 13.13 -1 2 0 410.32 13.10 -2 -2 0 100.48 3.36 2 -2 0 101.96 3.48 -2 -2 0 99.89 3.51 2 -2 0 95.41 3.43 2 -2 0 104.57 3.46 -2 -2 0 101.53 3.47 -2 -2 0 101.21 3.38 -2 2 0 102.26 3.44 -2 2 0 105.01 3.49 2 2 0 98.76 3.35 -2 2 0 100.18 3.46 2 2 0 100.15 3.51 -3 -2 0 133.47 4.68 3 -2 0 136.50 4.59 -3 -2 0 136.68 4.74 -3 -2 0 138.43 4.48 -3 -2 0 134.81 4.60 3 -2 0 143.15 4.71 3 -2 0 133.98 4.70 -3 2 0 139.53 4.71 3 2 0 136.86 4.69 3 2 0 135.75 4.75 -3 2 0 128.56 4.67 -3 2 0 141.10 4.60 3 2 0 132.67 4.56 4 -2 0 0.49 0.20 -4 -2 0 0.30 0.30 -4 -2 0 0.33 0.07 -4 -2 0 0.46 0.28 -4 -2 0 0.41 0.07 4 -2 0 0.52 0.38 -4 2 0 0.36 0.20 -4 2 0 -0.02 0.29 -4 2 0 0.44 0.41 4 2 0 0.28 0.23 4 2 0 0.55 0.38 5 -2 0 41.96 1.58 -5 -2 0 42.68 1.85 5 -2 0 39.38 1.85 5 2 0 40.91 1.93 -5 2 0 44.76 1.60 -5 2 0 42.33 1.85 5 2 0 41.38 1.68 6 -2 0 4.93 0.44 -6 -2 0 3.29 0.62 6 -2 0 4.71 0.72 6 2 0 4.12 0.76 6 2 0 5.02 0.63 -6 2 0 3.22 0.73 -7 -2 0 43.11 2.16 7 -2 0 39.00 2.02 -7 2 0 43.40 2.07 7 2 0 40.74 1.81 8 -2 0 -0.45 0.59 -8 -2 0 0.59 0.63 -8 2 0 0.42 0.63 8 2 0 0.36 0.52 9 -2 0 87.31 3.72 -9 -2 0 87.46 3.90 9 2 0 85.76 3.36 -9 2 0 89.25 3.92 -10 -2 0 -0.29 0.79 10 -2 0 0.55 0.85 -10 2 0 -1.47 1.05 -11 -2 0 22.15 1.94 11 -2 0 17.55 1.73 -11 2 0 19.38 1.87 -12 -2 0 -0.28 1.36 -12 2 0 1.87 1.43 0 -3 0 0.22 0.13 0 -3 0 0.12 0.13 0 -3 0 -0.13 0.18 0 3 0 0.30 0.21 0 3 0 0.39 0.14 0 3 0 -0.08 0.12 -1 -3 0 29.66 1.18 1 -3 0 27.53 1.08 1 -3 0 25.99 1.15 -1 -3 0 29.05 1.00 1 -3 0 27.39 1.11 -1 -3 0 27.96 1.10 1 3 0 28.95 1.18 1 3 0 27.99 0.98 1 3 0 28.48 0.97 1 3 0 28.31 1.12 -1 3 0 29.23 1.10 -1 3 0 27.43 1.09 -1 3 0 25.96 1.08 -1 3 0 29.79 1.15 2 -3 0 29.02 1.15 -2 -3 0 29.65 1.11 -2 -3 0 29.59 1.05 2 -3 0 27.42 1.19 -2 -3 0 28.47 1.21 2 -3 0 26.67 1.17 -2 3 0 28.69 1.17 -2 3 0 27.88 1.14 2 3 0 26.84 1.20 -2 3 0 28.19 1.17 2 3 0 27.51 0.99 -3 -3 0 12.09 0.58 -3 -3 0 10.52 0.69 -3 -3 0 10.64 0.73 3 -3 0 11.70 0.67 3 -3 0 11.21 0.67 -3 -3 0 10.95 0.54 3 -3 0 11.85 0.70 3 3 0 10.59 0.51 -3 3 0 11.17 0.73 3 3 0 9.83 0.77 -3 3 0 11.10 0.64 -3 3 0 10.83 0.72 -4 -3 0 6.01 0.69 -4 -3 0 5.60 0.34 4 -3 0 6.41 0.59 4 -3 0 5.68 0.50 -4 -3 0 5.67 0.48 4 3 0 5.29 0.60 -4 3 0 5.28 0.57 -4 3 0 6.06 0.52 4 3 0 6.07 0.45 -5 -3 0 0.57 0.39 5 -3 0 0.25 0.48 5 -3 0 0.78 0.27 -5 3 0 -0.05 0.50 5 3 0 0.37 0.29 5 3 0 1.17 0.53 -5 3 0 0.60 0.27 6 -3 0 6.43 0.54 6 -3 0 6.52 0.85 -6 -3 0 5.34 0.85 -6 3 0 5.57 0.53 6 3 0 6.87 0.81 -6 3 0 5.25 0.73 6 3 0 5.99 0.58 -7 -3 0 5.21 0.81 7 -3 0 3.33 0.48 7 -3 0 2.80 0.79 -7 3 0 3.45 0.87 7 3 0 3.59 0.86 7 3 0 4.64 0.60 -8 -3 0 2.35 0.96 8 -3 0 2.88 0.83 -8 3 0 2.81 0.78 8 3 0 2.07 0.51 -9 -3 0 13.66 1.68 9 -3 0 20.30 1.70 -9 3 0 15.32 1.46 -10 -3 0 6.86 1.23 10 -3 0 7.79 1.24 -10 3 0 6.51 1.20 11 -3 0 9.63 1.40 -11 -3 0 11.00 1.75 -11 3 0 13.53 1.80 -12 -3 0 0.81 1.41 -12 3 0 1.69 1.47 0 -4 0 133.62 4.72 0 -4 0 145.51 4.61 0 -4 0 136.00 4.59 0 4 0 138.07 4.73 0 4 0 134.87 4.58 0 4 0 138.38 4.59 1 -4 0 39.83 1.39 1 -4 0 34.52 1.45 1 -4 0 36.61 1.38 -1 -4 0 35.30 1.46 -1 -4 0 35.11 1.42 1 -4 0 35.62 1.37 -1 -4 0 36.52 1.28 1 4 0 35.86 1.44 1 4 0 35.47 1.24 1 4 0 36.92 1.24 -1 4 0 33.03 1.35 -1 4 0 34.44 1.36 -1 4 0 34.28 1.37 1 4 0 34.89 1.47 -1 4 0 34.89 1.46 2 -4 0 26.70 1.23 -2 -4 0 29.13 1.29 2 -4 0 28.91 1.22 2 -4 0 28.71 1.23 -2 -4 0 30.00 1.19 -2 -4 0 28.77 1.08 -2 4 0 28.68 1.21 -2 4 0 27.75 1.22 2 4 0 28.40 1.29 2 4 0 28.24 0.98 -2 4 0 30.18 1.23 -2 4 0 30.49 1.26 3 -4 0 17.56 0.95 -3 -4 0 18.27 0.81 3 -4 0 18.68 0.96 -3 -4 0 18.28 0.83 -3 -4 0 18.55 0.99 -3 4 0 16.94 0.92 3 4 0 16.36 1.04 -3 4 0 18.00 0.97 3 4 0 18.75 0.68 4 -4 0 130.96 4.82 4 -4 0 136.94 4.75 -4 -4 0 132.20 4.79 -4 -4 0 134.81 4.56 -4 -4 0 142.27 4.66 -4 4 0 134.52 4.80 4 4 0 132.02 4.50 -4 4 0 139.72 4.73 4 4 0 133.18 4.91 5 -4 0 9.35 0.72 -5 -4 0 11.33 0.98 5 -4 0 11.33 0.98 -5 -4 0 10.12 0.50 5 4 0 8.94 0.86 -5 4 0 10.63 0.96 5 4 0 10.18 0.56 -5 4 0 10.24 0.74 6 -4 0 74.77 2.86 -6 -4 0 71.95 3.14 6 -4 0 77.67 3.13 6 4 0 76.56 3.26 -6 4 0 79.14 2.88 -6 4 0 74.89 3.14 6 4 0 80.34 2.74 7 -4 0 11.31 1.23 7 -4 0 14.08 0.86 -7 -4 0 15.77 1.22 -7 4 0 11.10 1.30 7 4 0 15.14 0.80 7 4 0 12.74 1.37 8 -4 0 81.78 2.93 8 -4 0 75.73 3.47 -8 -4 0 80.96 3.56 -8 4 0 81.49 3.56 -9 -4 0 10.19 1.30 9 -4 0 8.21 1.22 -9 4 0 10.38 1.43 10 -4 0 51.48 2.82 -10 -4 0 50.11 2.81 -10 4 0 53.92 3.03 11 -4 0 5.68 1.36 -11 -4 0 8.74 1.67 -11 4 0 4.76 1.49 -12 -4 0 23.51 2.19 -12 4 0 20.24 2.49 0 -5 0 0.02 0.22 0 -5 0 -0.11 0.19 0 -5 0 0.07 0.19 0 5 0 0.16 0.29 0 5 0 -0.34 0.17 0 5 0 -0.02 0.17 0 5 0 0.13 0.21 -1 -5 0 22.52 1.04 -1 -5 0 19.75 0.96 1 -5 0 18.04 0.91 1 -5 0 19.71 0.93 1 -5 0 19.81 1.05 1 -5 0 20.75 0.90 -1 -5 0 18.53 0.80 -1 5 0 19.33 1.03 1 5 0 21.42 1.09 1 5 0 19.92 0.76 -1 5 0 19.30 0.70 -1 5 0 20.11 0.89 -1 5 0 19.91 0.90 1 5 0 18.88 0.76 1 5 0 20.05 1.01 -2 -5 0 41.46 1.67 2 -5 0 42.01 1.67 -2 -5 0 43.43 1.80 2 -5 0 39.81 1.75 2 -5 0 42.78 1.72 -2 -5 0 42.48 1.51 -2 5 0 43.21 1.74 2 5 0 42.00 1.68 -2 5 0 41.71 1.68 -2 5 0 36.92 1.62 -2 5 0 44.72 1.69 2 5 0 38.73 1.75 -3 -5 0 0.34 0.26 3 -5 0 0.52 0.35 3 -5 0 0.43 0.33 -3 -5 0 0.19 0.21 -3 5 0 0.42 0.32 -3 5 0 0.63 0.40 3 5 0 0.46 0.31 -4 -5 0 16.91 0.83 -4 -5 0 17.11 0.86 4 -5 0 17.19 1.04 4 -5 0 14.79 0.99 -4 -5 0 15.38 1.06 4 5 0 17.92 1.10 4 5 0 16.61 0.59 -4 5 0 18.28 1.00 -4 5 0 17.73 1.00 5 -5 0 9.57 0.83 -5 -5 0 11.21 0.62 -5 -5 0 11.36 0.90 5 -5 0 12.07 0.93 5 5 0 11.15 0.48 5 5 0 9.98 0.93 -5 5 0 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32.74 2.30 9 -4 -4 5.84 1.14 -9 -4 4 6.06 1.26 -9 4 4 6.20 1.24 9 4 -4 7.73 1.22 9 4 -4 7.23 1.17 -8 -4 4 36.93 2.24 8 -4 -4 40.77 1.73 8 -4 -4 42.26 2.42 8 4 -4 35.82 2.17 -8 4 4 37.70 2.09 8 4 -4 35.61 2.18 7 -4 -4 2.15 0.90 7 -4 -4 2.02 0.52 -7 -4 4 1.35 0.82 7 4 -4 1.67 0.59 -7 4 4 1.42 0.63 7 4 -4 2.11 0.75 -6 -4 4 60.32 2.73 6 -4 -4 65.22 2.63 6 -4 -4 62.21 2.81 -6 4 4 68.36 2.45 6 4 -4 64.53 2.32 6 4 -4 59.41 2.73 -6 4 4 59.89 2.71 6 4 -4 61.47 2.73 5 -4 -4 1.30 0.49 5 -4 -4 -0.39 0.57 5 -4 -4 0.97 0.44 -5 -4 4 0.58 0.54 5 4 -4 0.39 0.52 -5 4 4 1.20 0.56 5 4 -4 0.98 0.56 5 4 -4 0.65 0.28 -5 4 4 0.57 0.26 -4 -4 4 22.89 1.08 4 -4 -4 21.25 1.33 -4 -4 4 18.98 1.18 4 -4 -4 20.06 1.31 4 4 -4 19.81 1.31 -4 4 4 23.35 0.90 -4 4 4 21.28 1.19 4 4 -4 22.14 1.29 4 4 -4 22.55 1.28 4 4 -4 23.28 1.09 3 -4 -4 25.50 1.34 -3 -4 4 24.71 1.19 3 -4 -4 24.00 1.31 -3 -4 4 23.07 1.17 3 4 -4 23.66 1.38 -3 4 4 24.42 1.14 3 4 -4 24.69 1.28 3 4 -4 24.53 1.30 3 4 -4 25.52 1.18 -2 -4 4 17.76 1.07 2 -4 -4 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1.98 6 -5 -4 33.60 1.83 6 -5 -4 40.22 2.16 6 5 -4 40.32 1.99 -6 5 4 41.08 1.62 6 5 -4 35.86 2.05 6 5 -4 41.22 1.62 -6 5 4 39.58 2.00 5 -5 -4 6.67 0.89 -5 -5 4 6.76 0.84 -5 -5 4 5.72 0.63 5 -5 -4 7.50 0.87 5 -5 -4 7.49 0.82 5 5 -4 7.70 0.62 -5 5 4 7.33 0.50 -5 5 4 6.73 0.83 5 5 -4 6.50 0.84 5 5 -4 6.32 0.81 4 -5 -4 162.43 5.70 4 -5 -4 148.77 5.67 4 -5 -4 163.64 5.66 -4 -5 4 156.94 5.56 -4 -5 4 158.36 5.47 4 5 -4 163.25 5.72 4 5 -4 151.24 5.60 4 5 -4 151.35 5.76 -4 5 4 150.08 5.52 4 5 -4 162.93 5.49 -4 5 4 160.87 5.17 3 -5 -4 11.41 0.94 -3 -5 4 11.72 0.84 -3 -5 4 11.74 0.83 3 -5 -4 13.43 0.94 -3 5 4 13.74 0.86 3 5 -4 11.36 0.88 3 5 -4 12.89 0.86 3 5 -4 12.48 0.96 3 5 -4 11.69 0.96 2 -5 -4 25.14 1.23 2 -5 -4 25.46 1.12 2 -5 -4 23.33 1.18 -2 -5 4 22.97 1.18 2 5 -4 21.08 1.21 2 5 -4 23.89 1.32 -2 5 4 23.37 1.11 -2 5 4 25.44 1.10 -2 5 4 25.50 1.22 2 5 -4 21.98 1.22 2 5 -4 25.12 1.36 1 -5 -4 64.95 2.25 1 -5 -4 61.62 2.40 -1 -5 4 65.15 2.44 -1 -5 4 63.07 2.59 1 -5 -4 63.74 2.43 1 -5 -4 68.33 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7 -4 1.28 0.47 2 7 -4 0.56 0.41 -2 7 4 1.57 0.33 2 7 -4 0.84 0.45 -2 7 4 0.99 0.14 -2 7 4 0.59 0.38 -1 -7 4 103.54 3.96 -1 -7 4 106.80 3.73 1 -7 -4 106.84 3.78 1 -7 -4 103.57 3.70 -1 7 4 103.92 3.63 1 7 -4 103.13 3.88 1 7 -4 99.40 3.75 -1 7 4 108.01 3.72 -1 7 4 109.93 3.68 -1 7 4 106.74 3.60 0 -7 -4 0.67 0.27 0 -7 -4 0.63 0.29 0 -7 4 -0.10 0.48 0 -7 4 0.85 0.31 0 -7 -4 0.47 0.29 0 7 4 0.35 0.28 0 7 -4 0.03 0.27 0 7 -4 0.28 0.46 -1 -7 -4 143.26 4.79 1 -7 4 132.32 5.07 -1 -7 -4 136.89 4.90 -1 -7 -4 140.09 4.62 -1 7 -4 136.62 4.98 -1 7 -4 136.79 4.74 1 7 4 140.18 4.87 -2 -7 -4 7.78 0.69 2 -7 4 8.37 0.84 -2 7 -4 8.93 0.92 2 7 4 9.17 0.83 -2 7 -4 7.49 0.62 3 -7 4 75.03 3.22 -3 7 -4 81.30 3.18 -3 7 -4 74.81 2.97 3 7 4 79.58 3.13 -3 7 -4 78.96 2.90 -4 -7 -4 24.42 1.35 4 -7 4 24.96 1.56 -4 7 -4 21.86 1.49 4 7 4 24.04 1.55 -4 7 -4 22.83 1.33 -5 -7 -4 116.66 4.50 -5 -7 -4 120.51 4.05 5 -7 4 116.50 4.60 -5 7 -4 124.47 4.68 -5 7 -4 120.68 4.49 -6 -7 -4 12.04 1.24 6 -7 4 15.72 1.30 -6 7 -4 14.73 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1.32 -1 -12 -15 0.84 1.32 -1 12 -15 1.47 1.34 2 13 -15 3.54 1.43 1 13 -15 4.01 1.46 0 -13 -15 1.15 1.40 6 0 -16 4.11 1.76 5 0 -16 -0.72 1.50 5 0 -16 0.28 1.11 4 0 -16 -0.86 1.45 4 0 -16 -0.91 1.39 3 0 -16 0.44 1.43 3 0 -16 0.81 1.07 2 0 -16 33.37 2.72 2 0 -16 30.26 2.51 1 0 -16 0.84 1.45 1 0 -16 0.35 1.27 0 0 -16 56.98 3.37 0 0 -16 55.05 3.58 -1 0 -16 0.96 1.47 -1 0 -16 -0.07 1.25 -2 0 -16 24.66 2.61 -3 0 -16 -0.38 0.98 6 -1 -16 1.06 1.59 6 1 -16 0.04 1.28 5 -1 -16 -0.96 1.06 5 -1 -16 0.97 1.51 5 1 -16 -0.11 1.49 5 1 -16 4.46 1.76 4 -1 -16 3.28 1.64 4 -1 -16 3.08 1.56 4 1 -16 5.70 1.72 4 1 -16 3.98 1.69 3 -1 -16 0.12 1.48 3 -1 -16 -0.05 0.99 3 1 -16 1.00 1.10 3 1 -16 -1.89 0.92 2 -1 -16 3.71 1.43 2 -1 -16 2.98 1.26 2 1 -16 -0.14 1.35 2 1 -16 0.91 1.51 1 -1 -16 1.45 1.32 1 -1 -16 0.16 1.44 1 1 -16 0.45 1.07 1 1 -16 1.89 1.36 0 -1 -16 4.23 1.63 0 -1 -16 8.36 1.61 0 1 -16 6.98 1.67 0 1 -16 5.03 1.58 -1 -1 -16 0.35 1.39 -1 -1 -16 1.28 1.29 -1 1 -16 1.43 1.41 -1 1 -16 1.97 1.36 -2 -1 -16 10.27 1.89 -2 1 -16 11.67 1.68 -2 1 -16 11.01 1.86 -3 -1 -16 0.98 1.10 -3 1 -16 3.82 1.60 6 -2 -16 -0.80 1.53 5 -2 -16 7.55 1.69 5 -2 -16 6.19 1.82 5 2 -16 5.34 1.78 5 2 -16 7.71 1.86 4 -2 -16 3.03 1.35 4 -2 -16 3.16 1.56 4 2 -16 3.43 1.67 4 2 -16 2.03 1.24 3 -2 -16 11.60 1.83 3 -2 -16 10.60 2.03 3 2 -16 10.82 1.96 3 2 -16 10.07 1.92 2 -2 -16 3.72 1.32 2 -2 -16 4.76 1.50 2 2 -16 4.76 1.35 2 2 -16 5.05 1.61 1 -2 -16 22.55 2.56 1 -2 -16 20.32 2.24 1 2 -16 18.14 2.30 1 2 -16 18.37 2.25 0 -2 -16 2.88 1.21 0 2 -16 2.85 1.46 0 2 -16 2.46 1.19 -1 -2 -16 2.20 1.19 -1 2 -16 1.60 1.16 -1 2 -16 4.28 1.51 -2 -2 -16 3.98 1.60 -2 2 -16 1.38 1.47 -2 2 -16 5.27 1.61 -3 -2 -16 11.55 2.02 -3 2 -16 15.17 2.48 -3 2 -16 12.50 1.77 6 -3 -16 2.64 1.71 5 -3 -16 3.09 1.30 5 -3 -16 0.95 1.53 5 3 -16 3.66 1.64 5 3 -16 0.53 1.16 4 -3 -16 3.20 1.68 4 -3 -16 3.53 1.60 4 3 -16 5.24 1.71 4 3 -16 5.02 1.77 3 -3 -16 0.43 1.35 3 -3 -16 -0.72 1.41 3 3 -16 -0.33 1.03 3 3 -16 0.86 1.49 2 -3 -16 0.77 1.32 2 -3 -16 3.56 1.30 2 3 -16 2.11 1.14 2 3 -16 2.76 1.53 1 -3 -16 0.13 1.47 1 -3 -16 1.11 1.26 1 3 -16 0.30 0.99 1 3 -16 -0.78 0.96 0 -3 -16 1.15 1.13 0 -3 -16 0.10 1.15 0 3 -16 -0.15 1.39 0 3 -16 3.05 1.48 -1 -3 -16 1.21 1.12 -1 3 -16 2.75 1.43 -1 3 -16 1.53 1.49 -2 -3 -16 0.83 1.43 -2 3 -16 0.33 1.38 -2 3 -16 0.96 1.07 -3 -3 -16 5.92 2.05 -3 3 -16 4.79 1.67 -3 3 -16 5.79 1.70 6 -4 -16 17.50 2.42 5 -4 -16 -1.17 1.36 5 -4 -16 1.33 1.21 5 4 -16 0.00 1.46 5 4 -16 0.08 1.54 4 -4 -16 6.73 1.71 4 -4 -16 4.86 1.75 4 4 -16 6.03 1.50 4 4 -16 4.97 1.44 3 -4 -16 2.64 1.61 3 -4 -16 0.07 1.33 3 4 -16 -1.14 1.36 3 4 -16 1.88 1.53 2 -4 -16 9.73 1.73 2 -4 -16 12.19 1.77 2 4 -16 6.67 1.82 2 4 -16 7.05 1.49 1 -4 -16 0.91 1.50 1 -4 -16 1.75 1.31 1 4 -16 0.96 1.45 1 4 -16 0.57 1.38 0 -4 -16 5.17 1.39 0 4 -16 4.10 1.57 0 4 -16 4.75 1.64 -1 -4 -16 0.08 1.07 -1 4 -16 1.88 1.44 -1 4 -16 1.19 1.37 -2 -4 -16 0.40 1.43 -2 4 -16 1.66 1.50 -2 4 -16 1.39 1.50 -3 4 -16 -0.21 1.40 -3 4 -16 -0.69 0.98 -4 4 -16 2.18 1.62 6 -5 -16 0.69 1.32 5 -5 -16 0.83 1.45 5 -5 -16 3.20 1.67 5 5 -16 1.11 1.16 5 5 -16 1.43 1.40 4 -5 -16 1.97 1.49 4 -5 -16 4.36 1.73 4 5 -16 3.32 1.75 4 5 -16 1.91 1.55 3 -5 -16 2.17 1.43 3 -5 -16 1.62 1.52 3 5 -16 1.46 1.11 3 5 -16 3.99 1.70 2 -5 -16 2.05 1.35 2 -5 -16 3.24 1.27 2 5 -16 3.06 1.57 2 5 -16 1.82 1.22 1 -5 -16 -0.72 1.36 1 5 -16 -0.26 0.97 1 5 -16 0.36 1.47 0 -5 -16 0.04 1.39 0 5 -16 0.31 1.00 0 5 -16 -0.25 1.45 -1 -5 -16 1.13 1.40 -1 5 -16 3.11 1.22 -1 5 -16 1.56 1.49 -2 -5 -16 -1.04 1.38 -2 5 -16 0.20 1.44 -2 5 -16 1.18 1.11 -3 5 -16 -2.05 1.39 -3 5 -16 1.16 1.73 5 -6 -16 14.89 2.27 5 -6 -16 16.74 2.31 4 -6 -16 4.32 1.64 4 -6 -16 3.16 1.60 4 6 -16 2.84 1.61 4 6 -16 1.75 1.63 3 -6 -16 24.62 2.50 3 -6 -16 23.10 2.32 3 6 -16 28.27 2.76 3 6 -16 26.84 2.86 2 -6 -16 2.83 1.38 2 -6 -16 1.75 1.52 2 6 -16 1.68 1.45 2 6 -16 1.42 1.62 1 -6 -16 14.05 2.12 1 6 -16 22.05 2.63 1 6 -16 16.80 1.99 0 -6 -16 1.93 1.55 0 6 -16 1.54 1.65 0 6 -16 -0.36 1.35 -1 -6 -16 16.00 2.19 -1 6 -16 14.44 2.21 -1 6 -16 14.37 2.08 -2 -6 -16 0.56 1.47 -2 6 -16 0.38 1.05 -2 6 -16 -0.43 1.40 -3 6 -16 17.98 2.45 5 -7 -16 3.01 1.26 5 -7 -16 2.09 1.26 4 -7 -16 4.84 1.61 4 -7 -16 3.59 1.58 4 7 -16 3.73 1.34 4 7 -16 5.21 2.18 3 -7 -16 3.84 1.61 3 -7 -16 1.52 1.45 3 7 -16 1.70 1.34 3 7 -16 2.52 1.72 3 7 -16 1.66 1.55 2 -7 -16 0.81 1.48 2 7 -16 -0.17 1.49 2 7 -16 0.67 1.08 1 -7 -16 0.10 1.36 1 7 -16 -1.47 1.26 1 7 -16 -0.35 1.14 0 -7 -16 0.30 1.40 0 7 -16 1.69 1.48 0 7 -16 -0.07 1.12 -1 -7 -16 0.27 1.41 -1 7 -16 1.60 1.59 -1 7 -16 -0.03 1.40 -2 -7 -16 0.23 1.13 -2 7 -16 0.57 1.43 -2 7 -16 -1.61 1.51 -3 7 -16 7.91 2.31 5 -8 -16 5.97 1.78 5 -8 -16 6.91 2.06 4 -8 -16 12.29 2.02 4 -8 -16 13.85 2.14 4 8 -16 10.94 2.00 3 -8 -16 6.15 1.69 3 8 -16 4.69 1.54 3 8 -16 5.60 1.76 2 -8 -16 15.23 2.08 2 8 -16 8.87 1.65 2 8 -16 16.63 2.13 1 -8 -16 6.11 1.76 1 8 -16 10.93 1.99 1 8 -16 13.81 2.30 0 -8 -16 7.84 1.79 0 8 -16 7.33 1.78 0 8 -16 4.45 1.49 -1 -8 -16 3.98 1.54 -1 8 -16 3.83 1.59 -1 8 -16 2.73 1.68 -2 8 -16 9.12 2.43 -2 8 -16 7.93 1.84 4 -9 -16 -1.70 1.56 4 -9 -16 -0.56 1.28 3 -9 -16 4.37 1.62 3 9 -16 2.59 1.53 3 9 -16 3.20 1.53 2 -9 -16 0.24 1.39 2 9 -16 -0.28 0.97 1 -9 -16 1.11 1.33 1 9 -16 0.41 1.37 1 9 -16 1.57 2.00 0 -9 -16 -1.57 1.30 0 9 -16 0.68 1.98 0 9 -16 -0.93 1.31 -1 -9 -16 -0.80 1.36 -1 9 -16 0.26 1.45 3 -10 -16 3.97 1.49 3 10 -16 3.65 1.95 3 10 -16 1.89 1.21 2 -10 -16 8.03 1.80 2 10 -16 7.09 1.73 1 -10 -16 1.44 1.40 1 10 -16 1.94 1.39 0 -10 -16 5.83 1.70 0 10 -16 6.48 1.70 4 0 -17 -0.91 1.06 3 0 -17 10.42 1.99 2 0 -17 1.05 1.58 2 0 -17 0.87 1.43 1 0 -17 3.62 1.38 1 0 -17 3.49 1.55 0 0 -17 -0.59 1.32 0 0 -17 -0.12 1.33 -1 0 -17 0.36 1.84 4 -1 -17 1.30 1.16 4 1 -17 0.21 1.17 3 -1 -17 4.83 1.61 3 1 -17 5.09 1.44 2 -1 -17 2.60 1.52 2 -1 -17 1.39 1.27 2 1 -17 4.06 1.57 2 1 -17 2.07 1.67 1 -1 -17 8.92 1.79 1 -1 -17 7.13 1.96 1 1 -17 5.89 1.84 1 1 -17 11.66 1.89 0 -1 -17 8.25 2.33 0 -1 -17 9.75 1.59 0 1 -17 8.05 1.53 -1 1 -17 14.30 2.14 4 -2 -17 0.03 1.10 3 -2 -17 2.62 1.20 3 2 -17 6.05 1.83 2 -2 -17 0.33 1.19 2 -2 -17 1.34 1.10 2 2 -17 -0.90 0.97 2 2 -17 0.05 1.53 1 -2 -17 -1.31 1.48 1 -2 -17 -0.23 1.28 1 2 -17 -0.91 1.52 1 2 -17 -0.05 1.02 0 -2 -17 -0.06 1.84 0 2 -17 1.89 1.93 0 2 -17 1.83 1.45 -1 2 -17 -0.70 1.40 -2 2 -17 -0.20 1.38 4 -3 -17 -0.38 1.40 3 -3 -17 5.21 1.63 3 3 -17 2.93 1.78 2 -3 -17 4.51 1.65 2 -3 -17 7.47 1.65 2 3 -17 3.81 1.70 1 -3 -17 -1.17 1.55 1 -3 -17 1.10 1.43 1 3 -17 -1.30 1.23 1 3 -17 4.67 1.66 0 3 -17 4.33 1.67 -1 3 -17 3.38 1.67 -2 3 -17 8.49 1.88 4 -4 -17 0.28 1.49 3 -4 -17 1.70 1.45 3 4 -17 1.05 1.83 2 -4 -17 2.92 1.51 2 -4 -17 -0.37 1.29 2 4 -17 -1.48 1.46 1 -4 -17 2.34 1.97 1 4 -17 -1.89 1.41 0 4 -17 1.67 1.52 -1 4 -17 -0.49 1.41 4 -5 -17 -0.28 1.44 3 -5 -17 7.59 1.81 2 5 -17 1.28 2.09 1 5 -17 15.71 2.32 0 5 -17 9.46 2.09 -1 5 -17 5.44 1.81 3 -6 -17 1.21 1.48 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 25766 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_posn _atom_site_occupancy Ge Ge1 0.76188(2) 0.86320(2) 0.94053(2) 0.01395(6) Uani d . . 1 Cl Cl1 0.79992(5) 0.73029(3) 0.87531(4) 0.01460(9) Uani d . . 1 C C1 0.9848(2) 0.89044(11) 0.95740(17) 0.0123(3) Uani d . . 1 C C2 1.0576(2) 0.92870(11) 0.87184(17) 0.0129(3) Uani d . . 1 C C3 1.2136(2) 0.94726(12) 0.88968(18) 0.0159(4) Uani d . . 1 H H3 1.2623 0.9737 0.8313 0.019 Uiso calc U R 1 C C4 1.2978(2) 0.92705(13) 0.99292(18) 0.0172(4) Uani d . . 1 H H4 1.4039 0.939 1.0043 0.021 Uiso calc U R 1 C C5 1.2266(2) 0.88939(13) 1.07921(18) 0.0165(4) Uani d . . 1 H H5 1.2834 0.8755 1.1497 0.02 Uiso calc U R 1 C C6 1.0700(2) 0.87217(11) 1.06087(17) 0.0131(3) Uani d . . 1 C C7 0.9852(2) 0.83519(12) 1.14874(17) 0.0150(4) Uani d . . 1 H H7 1.0343 0.8225 1.2224 0.018 Uiso calc U R 1 C C8 0.7428(2) 0.78857(13) 1.20707(18) 0.0170(4) Uani d . . 1 C C9 0.8319(3) 0.75428(15) 1.3154(2) 0.0248(5) Uani d . . 1 H H9A 0.8989 0.7102 1.2947 0.037 Uiso calc U R 1 H H9B 0.76 0.7331 1.3665 0.037 Uiso calc U R 1 H H9C 0.8938 0.7976 1.3543 0.037 Uiso calc U R 1 C C10 0.6439(3) 0.85999(14) 1.2391(2) 0.0238(5) Uani d . . 1 H H10A 0.7083 0.9004 1.2823 0.036 Uiso calc U R 1 H H10B 0.5659 0.8401 1.2862 0.036 Uiso calc U R 1 H H10C 0.594 0.8851 1.1694 0.036 Uiso calc U R 1 C C11 0.6413(3) 0.72330(16) 1.1463(2) 0.0327(6) Uani d . . 1 H H11A 0.588 0.746 1.0761 0.049 Uiso calc U R 1 H H11B 0.5662 0.7048 1.1967 0.049 Uiso calc U R 1 H H11C 0.7045 0.6771 1.127 0.049 Uiso calc U R 1 C C12 0.9654(2) 0.94570(12) 0.76241(17) 0.0140(4) Uani d . . 1 H H12 1.0078 0.9752 0.7038 0.017 Uiso calc U R 1 C C13 0.7282(2) 0.93179(13) 0.63991(17) 0.0173(4) Uani d . . 1 C C14 0.8045(3) 0.97613(18) 0.5467(2) 0.0314(6) Uani d . . 1 H H14A 0.8359 1.0307 0.5737 0.047 Uiso calc U R 1 H H14B 0.732 0.9808 0.4779 0.047 Uiso calc U R 1 H H14C 0.8945 0.9454 0.5288 0.047 Uiso calc U R 1 C C15 0.6786(3) 0.84732(16) 0.5986(2) 0.0298(5) Uani d . . 1 H H15A 0.7681 0.8165 0.5797 0.045 Uiso calc U R 1 H H15B 0.605 0.852 0.5304 0.045 Uiso calc U R 1 H H15C 0.6307 0.8189 0.659 0.045 Uiso calc U R 1 C C16 0.5900(3) 0.9804(2) 0.6710(2) 0.0382(7) Uani d . . 1 H H16A 0.5462 0.9537 0.7346 0.057 Uiso calc U R 1 H H16B 0.513 0.983 0.6046 0.057 Uiso calc U R 1 H H16C 0.6223 1.0357 0.6936 0.057 Uiso calc U R 1 N N1 0.84271(19) 0.82061(10) 1.12295(14) 0.0135(3) Uani d . . 1 N N2 0.82777(19) 0.92002(10) 0.74786(14) 0.0140(3) Uani d . . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ge1 0.00892(10) 0.01544(10) 0.01725(11) 0.00030(7) 0.00021(7) -0.00292(8) Cl1 0.0140(2) 0.0141(2) 0.0152(2) -0.00023(16) -0.00082(16) -0.00676(16) C1 0.0120(8) 0.0111(8) 0.0137(9) 0.0005(6) 0.0009(7) -0.0026(6) C2 0.0127(9) 0.0117(8) 0.0143(9) 0.0010(6) 0.0017(7) -0.0017(7) C3 0.0130(9) 0.0144(9) 0.0204(10) -0.0016(7) 0.0021(7) 0.0004(7) C4 0.0116(9) 0.0188(9) 0.0209(10) -0.0033(7) -0.0007(7) -0.0021(8) C5 0.0136(9) 0.0180(9) 0.0171(10) -0.0006(7) -0.0025(7) -0.0014(7) C6 0.0125(8) 0.0130(8) 0.0138(9) -0.0006(6) 0.0007(7) -0.0017(7) C7 0.0171(9) 0.0152(9) 0.0124(9) 0.0018(7) 0.0001(7) 0.0000(7) C8 0.0180(10) 0.0184(9) 0.0152(9) -0.0027(7) 0.0046(7) 0.0031(7) C9 0.0280(12) 0.0265(11) 0.0208(11) 0.0039(9) 0.0068(9) 0.0093(9) C10 0.0199(11) 0.0284(11) 0.0246(11) 0.0047(9) 0.0100(9) 0.0083(9) C11 0.0422(15) 0.0317(13) 0.0249(12) -0.0201(11) 0.0071(11) 0.0016(10) C12 0.0159(9) 0.0128(8) 0.0136(9) 0.0008(7) 0.0032(7) 0.0003(7) C13 0.0151(9) 0.0229(10) 0.0134(9) 0.0012(7) -0.0008(7) 0.0008(7) C14 0.0274(13) 0.0467(15) 0.0188(11) -0.0041(11) -0.0042(9) 0.0137(10) C15 0.0338(14) 0.0333(13) 0.0201(11) -0.0065(10) -0.0086(10) -0.0033(9) C16 0.0282(13) 0.0616(19) 0.0232(13) 0.0242(13) -0.0055(10) -0.0058(12) N1 0.0138(8) 0.0138(7) 0.0131(8) -0.0004(6) 0.0021(6) 0.0013(6) N2 0.0145(8) 0.0148(8) 0.0127(8) 0.0023(6) 0.0009(6) -0.0009(6) 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' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 Ge1 N1 76.68(7) C1 Ge1 Cl1 93.95(5) N1 Ge1 Cl1 88.94(4) C6 C1 C2 118.71(18) C6 C1 Ge1 118.14(14) C2 C1 Ge1 123.12(15) C1 C2 C3 120.33(19) C1 C2 C12 117.54(17) C3 C2 C12 122.10(18) C4 C3 C2 120.17(19) C5 C4 C3 120.13(19) C4 C5 C6 119.13(19) C1 C6 C5 121.50(18) C1 C6 C7 115.92(18) C5 C6 C7 122.57(18) N1 C7 C6 117.81(18) N1 C8 C11 107.14(17) N1 C8 C10 106.46(16) C11 C8 C10 109.5(2) N1 C8 C9 113.40(17) C11 C8 C9 110.86(19) C10 C8 C9 109.36(18) N2 C12 C2 118.86(18) N2 C13 C15 106.30(17) N2 C13 C14 114.38(18) C15 C13 C14 109.8(2) N2 C13 C16 106.16(17) C15 C13 C16 110.1(2) C14 C13 C16 110.0(2) C7 N1 C8 122.67(17) C7 N1 Ge1 111.41(13) C8 N1 Ge1 125.60(13) C12 N2 C13 122.80(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ge1 C1 2.0004(19) Ge1 N1 2.2981(17) Ge1 Cl1 2.3477(5) C1 C6 1.394(3) C1 C2 1.396(3) C2 C3 1.400(3) C2 C12 1.475(3) C3 C4 1.395(3) C4 C5 1.391(3) C5 C6 1.400(3) C6 C7 1.466(3) C7 N1 1.281(3) C8 N1 1.485(2) C8 C11 1.524(3) C8 C10 1.530(3) C8 C9 1.532(3) C12 N2 1.277(3) C13 N2 1.479(3) C13 C15 1.518(3) C13 C14 1.527(3) C13 C16 1.529(3)