#------------------------------------------------------------------------------ #$Date: 2021-10-20 02:22:01 +0300 (Wed, 20 Oct 2021) $ #$Revision: 270041 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708588.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_7708588 loop_ _publ_author_name 'Henry, Andrew Timothy' 'Cosby, Taylor P. L.' 'Boyle, Paul D.' 'Baines, Kim M.' _publ_section_title ; Assessing the Lewis Acidity and Catalytic Activity of Bis(catecholato)germanes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03180E _journal_year 2021 _chemical_formula_sum 'C36 H56 Ge O6' _chemical_formula_weight 657.39 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2021-06-15 deposited with the CCDC. 2021-10-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.130(14) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.091(2) _cell_length_b 18.355(5) _cell_length_c 12.889(5) _cell_measurement_reflns_used 9916 _cell_measurement_temperature 110 _cell_measurement_theta_max 31.86 _cell_measurement_theta_min 2.73 _cell_volume 1673.2(9) _computing_cell_refinement SAINT _computing_data_collection Apex3 _computing_data_reduction SAINT _computing_molecular_graphics Mercury _computing_publication_material cif2tables.py _computing_structure_refinement SHELXL _computing_structure_solution SHELXT _diffrn_ambient_temperature 110 _diffrn_detector 'CCD plate' _diffrn_detector_type 'Bruker Apex2' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Kappa Axis Apex2' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 56754 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.841 _diffrn_reflns_theta_min 2.727 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_correction_T_min 0.6334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.305 _exptl_crystal_description plate _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.294 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.043 _refine_diff_density_max 2.679 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 202 _refine_ls_number_reflns 6714 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0487 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+1.9778P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1103 _refine_ls_wR_factor_ref 0.1195 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5108 _reflns_number_total 6714 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03180e3.cif _cod_data_source_block b20002 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7708588 _shelx_shelxl_version_number 2016/6 _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 0.766 _shelx_estimated_absorpt_t_max 0.960 _shelx_res_file ; TITL b20002 in P2(1)/c b20002.res created by SHELXL-2016/6 at 11:41:12 on 25-Aug-2020 CELL 0.71073 7.09101 18.35500 12.88868 90.0000 94.1304 90.0000 ZERR 2 0.00218 0.00469 0.00512 0.0000 0.0135 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O GE UNIT 72 112 12 2 TEMP -163.170 SIZE 0.043 0.153 0.294 ACTA REM omit reflections blocked by the beamstop OMIT 0 1 1 OMIT 0 2 0 L.S. 12 FMAP 2 PLAN 20 BOND $H CONF REM Instructions for potential hydrogen bonds HTAB C15 O2 WGHT 0.045800 1.977800 FVAR 0.55412 GE1 4 0.500000 0.500000 0.500000 10.50000 0.01856 0.01370 = 0.00837 0.00010 0.00067 -0.00022 O1 3 0.407340 0.589173 0.459857 11.00000 0.02277 0.01505 = 0.00894 0.00051 0.00011 0.00182 O2 3 0.422459 0.463574 0.371816 11.00000 0.02107 0.01372 = 0.00812 0.00042 0.00033 -0.00006 O3 3 0.766207 0.530434 0.450133 11.00000 0.02097 0.01899 = 0.01413 -0.00144 0.00499 -0.00346 C1 1 0.361623 0.588274 0.355054 11.00000 0.01362 0.01702 = 0.00822 0.00018 0.00094 0.00025 C2 1 0.365490 0.520010 0.307276 11.00000 0.01446 0.01460 = 0.01050 0.00158 0.00230 -0.00044 C3 1 0.318707 0.512429 0.200050 11.00000 0.01340 0.01590 = 0.01202 0.00049 0.00194 -0.00006 C4 1 0.278690 0.577290 0.144400 11.00000 0.01544 0.01739 = 0.01106 0.00096 0.00062 0.00137 AFIX 43 H4 2 0.247157 0.573910 0.071664 11.00000 -1.20000 AFIX 0 C5 1 0.282753 0.646345 0.190151 11.00000 0.01413 0.01649 = 0.01245 0.00210 0.00205 0.00084 C6 1 0.323291 0.651114 0.298295 11.00000 0.01665 0.01497 = 0.01250 0.00057 0.00134 0.00102 AFIX 43 H6 2 0.324339 0.697124 0.332090 11.00000 -1.20000 AFIX 0 C7 1 0.312058 0.436932 0.147416 11.00000 0.01832 0.01266 = 0.00988 -0.00029 0.00083 -0.00134 C8 1 0.260154 0.441709 0.030272 11.00000 0.02363 0.02126 = 0.01329 -0.00201 0.00112 -0.00012 AFIX 137 H8A 2 0.355053 0.470929 -0.002548 11.00000 -1.50000 H8B 2 0.135753 0.464654 0.018015 11.00000 -1.50000 H8C 2 0.256425 0.392604 0.000343 11.00000 -1.50000 AFIX 0 C9 1 0.159696 0.390778 0.196342 11.00000 0.03312 0.02364 = 0.01758 -0.00339 0.00664 -0.01000 AFIX 137 H9A 2 0.158095 0.341658 0.166492 11.00000 -1.50000 H9B 2 0.035614 0.413577 0.181881 11.00000 -1.50000 H9C 2 0.188607 0.387786 0.271727 11.00000 -1.50000 AFIX 0 C10 1 0.502924 0.398778 0.164247 11.00000 0.02775 0.02181 = 0.01633 -0.00278 0.00101 0.00729 AFIX 137 H10A 2 0.495382 0.350538 0.131627 11.00000 -1.50000 H10B 2 0.536097 0.393446 0.238995 11.00000 -1.50000 H10C 2 0.599913 0.427839 0.132933 11.00000 -1.50000 AFIX 0 C11 1 0.258428 0.716713 0.126465 11.00000 0.02250 0.01547 = 0.01455 0.00327 0.00201 0.00300 C12 1 0.139065 0.772840 0.181341 11.00000 0.03848 0.02257 = 0.02334 0.00303 0.00508 0.01135 AFIX 137 H12A 2 0.132055 0.818152 0.141030 11.00000 -1.50000 H12B 2 0.197746 0.782606 0.251129 11.00000 -1.50000 H12C 2 0.011318 0.753536 0.186840 11.00000 -1.50000 AFIX 0 C13 1 0.160540 0.703558 0.018396 11.00000 0.03952 0.02500 = 0.01829 0.00422 -0.00640 0.00280 AFIX 137 H13A 2 0.238177 0.670909 -0.021008 11.00000 -1.50000 H13B 2 0.144195 0.750097 -0.018422 11.00000 -1.50000 H13C 2 0.036549 0.681241 0.025398 11.00000 -1.50000 AFIX 0 C14 1 0.454792 0.748782 0.113362 11.00000 0.03076 0.02233 = 0.02743 0.00816 0.00426 -0.00321 AFIX 137 H14A 2 0.528295 0.714677 0.073899 11.00000 -1.50000 H14B 2 0.519995 0.757041 0.181998 11.00000 -1.50000 H14C 2 0.441681 0.795137 0.075807 11.00000 -1.50000 AFIX 0 C15 1 0.840714 0.507905 0.352533 11.00000 0.02063 0.02719 = 0.01867 -0.00394 0.00714 0.00043 AFIX 23 H15A 2 0.765066 0.467400 0.320390 11.00000 -1.20000 H15B 2 0.973921 0.491937 0.364117 11.00000 -1.20000 AFIX 0 C16 1 0.825684 0.575446 0.283791 11.00000 0.01909 0.03679 = 0.01627 0.00309 0.00379 -0.00386 AFIX 23 H16A 2 0.706688 0.574966 0.238632 11.00000 -1.20000 H16B 2 0.933785 0.578404 0.239460 11.00000 -1.20000 AFIX 0 C17 1 0.828319 0.639785 0.360866 11.00000 0.02032 0.02425 = 0.02603 0.00657 0.00163 -0.00342 AFIX 23 H17A 2 0.939783 0.671284 0.353175 11.00000 -1.20000 H17B 2 0.712289 0.669568 0.349414 11.00000 -1.20000 AFIX 0 C18 1 0.838280 0.604347 0.467655 11.00000 0.02593 0.02249 = 0.01993 -0.00157 0.00345 -0.00709 AFIX 23 H18A 2 0.970229 0.603256 0.498476 11.00000 -1.20000 H18B 2 0.759433 0.631337 0.515035 11.00000 -1.20000 AFIX 0 HKLF 4 REM b20002 in P2(1)/c REM R1 = 0.0487 for 5108 Fo > 4sig(Fo) and 0.0718 for all 6714 data REM 202 parameters refined using 0 restraints END WGHT 0.0458 1.9778 REM Highest difference peak 2.679, deepest hole -0.678, 1-sigma level 0.089 Q1 1 0.3618 0.7246 0.3569 11.00000 0.05 2.68 Q2 1 0.3694 0.5585 0.3273 11.00000 0.05 0.54 Q3 1 1.0000 0.5000 0.5000 10.50000 0.05 0.51 Q4 1 0.6311 0.7726 0.1399 11.00000 0.05 0.51 Q5 1 0.3035 0.5416 0.1694 11.00000 0.05 0.47 Q6 1 0.9664 0.5034 0.2218 11.00000 0.05 0.43 Q7 1 0.3152 0.6132 0.3268 11.00000 0.05 0.43 Q8 1 0.2739 0.6099 0.1778 11.00000 0.05 0.41 Q9 1 0.5207 0.5614 0.4760 11.00000 0.05 0.41 Q10 1 0.3961 0.4295 0.1475 11.00000 0.05 0.41 Q11 1 0.4518 0.5589 0.5113 11.00000 0.05 0.40 Q12 1 0.3318 0.5150 0.2562 11.00000 0.05 0.40 Q13 1 0.0633 0.7536 0.1426 11.00000 0.05 0.39 Q14 1 0.2787 0.6865 0.1621 11.00000 0.05 0.39 Q15 1 0.2977 0.6484 0.2430 11.00000 0.05 0.39 Q16 1 0.3187 0.4589 0.1672 11.00000 0.05 0.39 Q17 1 0.2119 0.7111 0.0839 11.00000 0.05 0.37 Q18 1 0.4249 0.5509 0.4824 11.00000 0.05 0.36 Q19 1 0.3321 0.4979 0.4781 11.00000 0.05 0.35 Q20 1 0.2652 0.4222 0.1607 11.00000 0.05 0.33 ; _shelx_res_checksum 1696 _shelx_hkl_file ; 1 0 0 4811.90 114.273 8 1 0 0 4913.81 112.703 1 1 0 0 4987.55 112.763 1 2 0 0 1512.86 36.5645 1 2 0 0 1593.97 36.7112 1 2 0 0 1500.50 39.8876 8 3 0 0 1689.90 40.5363 1 -3 0 0 1676.79 44.9306 5 3 0 0 1670.02 40.1528 6 3 0 0 1651.78 40.4126 1 3 0 0 1710.50 45.7486 8 -3 0 0 1695.81 44.1226 3 4 0 0 278.990 8.98920 1 4 0 0 295.644 15.1883 8 4 0 0 300.033 9.49061 6 -4 0 0 293.703 12.6003 4 -4 0 0 262.231 14.0365 5 4 0 0 279.395 9.56238 2 -4 0 0 277.045 13.1698 3 -5 0 0 262.084 13.3818 4 -5 0 0 243.680 15.2479 5 -5 0 0 267.563 14.1439 3 5 0 0 236.986 9.52999 6 5 0 0 278.428 16.4798 8 5 0 0 247.177 8.01788 1 5 0 0 238.439 9.22936 2 5 0 0 244.949 9.42267 6 6 0 0 743.212 21.1090 2 6 0 0 758.930 22.2886 6 -6 0 0 745.791 28.6569 3 -6 0 0 741.377 30.2982 5 -6 0 0 799.354 27.8982 4 6 0 0 705.783 31.0855 8 7 0 0 -8.9480 8.37798 8 -7 0 0 -1.7883 7.65653 3 7 0 0 4.47751 4.65009 6 -7 0 0 -3.9858 7.39318 5 -7 0 0 -3.9710 7.31001 4 8 0 0 75.3861 8.65201 6 8 0 0 59.1891 15.3319 8 -8 0 0 95.6069 15.5815 3 -8 0 0 55.1878 12.5844 5 9 0 0 356.902 30.1760 8 9 0 0 308.536 17.2473 6 -9 0 0 349.888 26.8097 5 -9 0 0 332.607 25.4419 3 -10 0 0 15.9648 14.4296 3 -10 0 0 4.14586 13.4242 5 10 0 0 15.3953 8.28720 6 -11 0 0 -1.1602 15.8110 3 -11 0 0 16.2076 16.0218 5 11 0 0 11.7410 9.69613 6 0 -1 0 -0.0435 0.44815 1 0 1 0 -0.3886 0.28061 1 1 -1 0 1017.62 23.7160 7 1 -1 0 995.033 24.2445 1 1 -1 0 950.151 25.2753 8 1 -1 0 1000.71 24.2653 1 -1 1 0 974.327 24.2325 1 -1 1 0 1031.20 23.5648 7 1 1 0 984.983 24.8038 8 2 -1 0 949.297 23.1898 1 2 -1 0 902.351 25.8345 8 2 -1 0 904.922 22.9869 1 2 1 0 873.337 21.4038 1 -2 1 0 878.806 22.9933 1 2 1 0 932.261 21.3914 1 2 1 0 902.464 25.2674 8 3 -1 0 48.4343 3.81450 6 3 -1 0 47.7109 6.60938 8 3 -1 0 56.5133 4.38743 1 -3 -1 0 55.1734 6.52497 3 -3 -1 0 44.4743 5.74046 5 3 -1 0 46.7237 3.88518 1 -3 1 0 54.5103 4.21162 1 -3 1 0 51.3877 6.25616 5 3 1 0 43.7104 2.57351 1 3 1 0 48.9794 6.31809 8 -3 1 0 48.2648 5.93037 3 4 -1 0 65.3770 5.12556 6 -4 -1 0 65.5057 7.62161 5 4 -1 0 75.5914 5.27309 2 -4 -1 0 83.2997 8.21778 3 4 -1 0 65.7386 5.01385 1 -4 -1 0 82.1730 7.76289 4 4 -1 0 66.3958 8.34804 8 4 1 0 78.1432 8.73592 8 -4 1 0 89.4929 7.84539 4 4 1 0 67.4450 2.64436 1 4 1 0 67.7030 3.91124 6 -4 1 0 69.9355 5.17287 1 -4 1 0 74.0024 8.18321 3 -4 1 0 63.7765 7.54732 5 4 1 0 70.0906 2.57258 1 5 -1 0 19.5290 3.42325 1 5 -1 0 10.8430 3.25821 6 -5 -1 0 17.9213 6.14083 3 5 -1 0 17.9326 3.62129 2 -5 -1 0 11.8451 5.87997 5 5 -1 0 21.3768 6.82482 8 -5 -1 0 23.5749 5.94133 4 5 1 0 18.2340 3.27184 6 5 1 0 11.3970 2.79592 6 -5 1 0 19.5760 6.11820 3 -5 1 0 20.0119 6.45073 5 5 1 0 23.5455 6.86002 8 5 1 0 14.7633 2.83892 2 -5 1 0 13.0245 5.60613 4 -6 -1 0 44.4650 9.43712 5 6 -1 0 45.9200 5.57941 1 6 -1 0 49.5153 5.58998 2 -6 -1 0 70.4336 9.77647 4 -6 -1 0 43.7465 9.07568 3 6 -1 0 60.5553 10.8986 8 6 -1 0 55.1227 6.15180 6 -6 1 0 55.0864 10.6370 5 6 1 0 47.7198 10.3988 8 6 1 0 53.6468 5.38614 6 -6 1 0 68.4562 9.46756 4 -6 1 0 48.8653 9.38266 3 -7 -1 0 19.8828 9.11539 5 7 -1 0 29.7523 11.7590 8 -7 -1 0 16.1753 8.55472 3 -7 -1 0 5.60339 8.00107 4 7 -1 0 16.6264 5.53274 6 7 1 0 20.5711 5.01309 6 -7 1 0 13.5428 8.72113 3 -7 1 0 20.0022 8.02028 4 7 1 0 26.8694 10.8160 8 -7 1 0 -1.5978 7.43631 5 -8 -1 0 4.04252 9.42967 5 -8 -1 0 -12.104 8.25714 4 8 -1 0 21.4894 12.7078 8 8 -1 0 2.71308 5.33937 6 -8 -1 0 -4.6503 8.61835 3 8 1 0 -1.8457 11.2050 8 -8 1 0 2.87544 9.56188 3 -8 1 0 -6.7516 8.14765 5 8 1 0 4.59353 5.27095 6 9 -1 0 26.1331 8.25795 6 -9 -1 0 12.5447 11.3770 5 9 -1 0 19.7039 14.4609 8 -9 -1 0 12.2447 11.4781 3 -9 1 0 6.92363 10.5747 5 9 1 0 16.3548 6.99434 6 -9 1 0 4.60554 12.2582 3 9 1 0 17.2494 14.0087 8 -10 -1 0 -10.065 11.9452 3 -10 -1 0 -1.9875 10.6158 5 10 -1 0 2.46412 8.42101 6 -10 1 0 -1.6389 12.1934 5 10 1 0 -15.433 6.82437 6 -10 1 0 -2.1849 13.2913 3 11 -1 0 8.06144 9.90819 6 -11 -1 0 5.30739 14.5644 5 11 1 0 -6.4574 8.48328 6 -11 1 0 14.0335 16.0856 3 -11 1 0 11.5941 15.6013 5 0 -2 0 5282.29 122.217 1 1 -2 0 3026.98 71.7809 8 1 -2 0 3122.45 71.2176 1 1 -2 0 2705.84 69.3291 7 1 2 0 3053.62 69.7810 1 1 2 0 3079.44 70.6753 8 -1 2 0 2868.41 69.3944 7 -1 2 0 3097.42 71.2549 1 1 2 0 3177.50 69.8228 1 2 -2 0 21.8716 3.33907 1 2 -2 0 21.5220 4.13713 8 2 2 0 11.9902 3.33389 8 -2 2 0 15.6111 2.81166 1 3 -2 0 45.8595 4.61814 1 3 -2 0 50.1099 4.44530 6 -3 -2 0 57.0898 6.20610 5 3 -2 0 51.0043 6.99367 8 -3 -2 0 43.7543 5.69426 4 3 2 0 43.0541 5.78234 8 -3 2 0 44.0854 6.04283 3 -3 2 0 48.0107 5.74290 5 -3 2 0 38.5276 4.25994 1 -4 -2 0 287.737 13.0536 4 4 -2 0 273.753 10.6670 1 -4 -2 0 285.965 14.3157 5 4 -2 0 283.168 10.7552 6 4 -2 0 296.311 10.7872 2 4 -2 0 283.235 15.4503 8 4 -2 0 285.334 10.4679 1 -4 -2 0 300.698 13.2301 3 -4 2 0 275.118 13.5902 3 -4 2 0 320.054 12.7320 4 4 2 0 293.309 14.5146 8 4 2 0 288.193 7.93012 6 -4 2 0 285.862 14.2450 5 -4 2 0 294.190 11.0175 1 4 2 0 260.268 8.00153 6 -5 -2 0 119.659 10.6799 4 5 -2 0 113.087 6.93612 2 -5 -2 0 94.1596 10.6069 5 5 -2 0 77.8712 10.9952 8 5 -2 0 102.681 6.66139 1 5 -2 0 104.224 7.23745 6 -5 -2 0 85.3360 9.72633 3 5 2 0 89.0113 5.16060 6 5 2 0 86.3300 4.22034 2 -5 2 0 103.398 11.3463 5 -5 2 0 100.097 10.8250 3 -5 2 0 112.347 9.66286 4 5 2 0 104.378 10.8575 8 5 2 0 96.0216 4.92760 6 -6 -2 0 209.342 16.1239 5 -6 -2 0 192.151 13.8207 4 6 -2 0 213.348 9.29436 1 6 -2 0 181.919 9.57972 2 -6 -2 0 193.992 14.2594 3 6 -2 0 172.831 16.7168 8 6 -2 0 206.823 11.0464 6 6 2 0 199.403 16.4414 8 -6 2 0 228.909 15.6939 3 6 2 0 199.409 8.52084 6 -6 2 0 199.409 16.4174 5 -6 2 0 212.661 13.6936 4 -7 -2 0 172.277 17.3960 5 -7 -2 0 211.913 16.4606 3 -7 -2 0 206.935 17.3165 4 7 -2 0 190.050 13.3145 2 7 -2 0 181.094 19.5769 8 7 -2 0 202.968 12.2272 6 -7 2 0 174.922 17.3916 5 7 2 0 181.268 18.7522 8 7 2 0 176.411 9.71032 6 -7 2 0 214.904 17.5420 3 -8 -2 0 81.3207 14.6567 5 8 -2 0 81.0398 10.2241 6 8 -2 0 108.033 18.4832 8 -8 -2 0 111.031 16.3977 3 -8 -2 0 87.8788 14.2900 4 8 2 0 68.9401 15.2174 8 8 2 0 66.2039 7.71617 6 -8 2 0 60.1718 13.7141 3 -8 2 0 87.6652 14.9150 5 9 -2 0 76.9966 18.4611 8 9 -2 0 107.554 11.8855 6 -9 -2 0 94.8003 16.8268 3 -9 -2 0 75.2736 15.9300 5 9 2 0 110.906 20.5801 8 -9 2 0 71.6525 15.9009 3 9 2 0 89.8123 9.64956 6 -9 2 0 81.5127 16.3608 5 -10 -2 0 74.9357 17.9821 3 10 -2 0 59.3685 11.5519 6 -10 -2 0 59.8621 17.2866 5 10 2 0 55.4535 9.70050 6 -10 2 0 50.0842 16.2636 3 -10 2 0 42.4873 14.9404 5 -11 -2 0 31.2352 16.7893 5 11 -2 0 53.5108 12.1507 6 -11 2 0 40.5680 17.5676 3 11 2 0 29.5988 9.82236 6 -11 2 0 19.6612 16.9598 5 0 -3 0 0.61727 1.77592 1 0 -3 0 1.99470 1.04489 8 0 3 0 2.23799 1.52257 1 -1 -3 0 3382.80 78.2595 1 1 -3 0 3206.58 79.5779 8 1 -3 0 3409.95 79.7154 1 -1 3 0 3325.91 79.6345 1 1 3 0 3404.70 78.2262 1 -1 3 0 3198.46 77.4084 7 1 3 0 3371.25 77.9963 8 1 3 0 3492.50 78.2357 1 2 -3 0 3052.81 78.2484 8 2 -3 0 3262.99 76.7334 1 2 3 0 3112.59 76.5596 8 2 3 0 3302.63 73.7034 1 -2 3 0 3183.49 73.8535 7 2 3 0 3171.61 73.6351 1 -2 3 0 3214.10 76.7247 1 3 -3 0 96.4973 8.86714 8 3 -3 0 94.2649 6.29174 6 3 -3 0 103.584 6.52051 2 -3 -3 0 96.8281 7.69781 5 -3 -3 0 113.363 8.04379 4 3 -3 0 98.9877 6.75882 1 -3 3 0 92.4331 7.62959 3 -3 3 0 104.995 8.21107 5 3 3 0 97.5184 7.57257 8 -3 3 0 110.745 6.54221 1 4 -3 0 474.223 15.6945 1 4 -3 0 493.055 15.6482 2 -4 -3 0 485.287 17.9103 4 -4 -3 0 469.207 17.4880 3 4 -3 0 444.769 20.0437 8 4 -3 0 475.212 15.6613 6 -4 -3 0 458.282 18.3986 5 -4 3 0 475.679 18.8849 5 -4 3 0 449.330 18.3340 3 4 3 0 468.068 18.6889 8 4 3 0 464.306 11.3314 6 4 3 0 465.001 11.3453 6 -4 3 0 458.350 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260.890 14.7472 8 -1 7 7 255.642 13.7066 2 1 7 -7 262.748 13.8864 2 -1 7 7 260.404 14.7465 7 1 7 -7 288.613 15.0758 1 1 7 -7 263.272 14.0866 6 -1 7 7 286.132 14.0788 5 -1 7 7 220.627 13.6434 1 0 -7 -7 2000.67 55.8228 4 0 -7 7 2036.99 55.4227 7 0 -7 -7 2040.96 57.3612 8 0 -7 7 2014.22 57.0350 1 0 -7 7 1987.19 55.8111 2 0 -7 -7 1997.34 56.1895 1 0 -7 -7 2090.14 55.5555 2 0 7 -7 1959.70 55.5240 2 0 7 7 1962.63 55.6066 1 0 7 7 2028.92 57.0371 7 0 7 7 2008.48 54.9204 2 0 7 -7 2091.94 57.4918 1 0 7 -7 2043.92 57.1899 8 0 7 7 2052.54 55.2295 6 -1 -7 -7 135.756 11.5738 8 -1 -7 -7 153.175 11.3318 4 -1 -7 -7 142.839 10.6906 1 1 -7 7 128.061 9.71716 7 1 -7 7 160.806 11.4271 2 1 -7 7 140.207 11.3945 6 1 -7 7 135.623 12.1941 1 -1 7 -7 141.828 11.7074 8 1 7 7 144.109 9.81748 2 -1 7 -7 152.043 10.6572 2 1 7 7 166.955 10.2582 6 -1 7 -7 158.446 9.17991 3 -1 7 -7 145.906 11.0698 1 1 7 7 148.619 11.5342 7 1 7 7 138.470 9.89060 1 2 -7 7 27.0262 6.81602 2 2 -7 7 10.9770 5.32127 6 -2 -7 -7 17.4842 6.48236 3 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52.9383 12.1052 8 -6 8 7 56.7027 12.9433 3 -5 -8 7 14.4158 8.67952 5 5 -8 -7 21.4496 8.32709 1 5 -8 -7 20.0716 8.12840 2 5 -8 -7 15.9470 8.05307 6 5 -8 -7 10.3839 10.7742 8 -5 -8 7 3.63247 8.32842 4 -5 8 7 3.68427 8.08199 3 -5 8 7 19.7018 8.24814 5 5 8 -7 4.73395 5.52289 1 5 8 -7 15.3998 7.34752 6 5 8 -7 3.80612 5.49561 2 5 8 -7 13.2008 8.67586 8 -5 8 7 9.06840 7.03627 1 -5 8 7 21.6923 7.51654 7 4 -8 -7 122.728 13.4152 6 -4 -8 7 117.175 12.8984 4 4 -8 -7 138.859 15.6304 8 -4 -8 7 114.927 12.8374 5 4 -8 -7 130.074 13.5232 2 4 -8 -7 124.709 13.6461 1 4 8 -7 124.693 11.7944 2 -4 8 7 121.344 12.3095 7 -4 8 7 132.034 14.3343 3 4 8 -7 119.988 12.9374 8 -4 8 7 126.856 13.1919 5 -4 8 7 150.041 13.6083 2 4 8 -7 143.323 12.9433 6 -4 8 7 144.381 13.9874 1 4 8 -7 125.704 12.0910 1 -3 -8 7 123.588 13.0531 2 3 -8 -7 135.085 13.7645 2 3 -8 -7 119.790 13.1925 1 -3 -8 7 129.901 12.5879 1 -3 -8 7 130.345 12.6551 4 3 -8 -7 105.238 11.5538 4 3 -8 -7 129.042 14.6222 8 -3 -8 7 146.713 13.4095 5 -3 -8 7 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54.1379 8.80433 4 2 -4 9 64.5262 8.76095 2 -2 -4 -9 43.4461 9.64816 8 2 -4 9 39.9722 7.92603 6 2 -4 9 64.2330 8.71728 7 -2 4 -9 76.0199 11.8253 8 2 4 9 73.0500 8.94954 6 -2 4 -9 57.2470 8.43741 3 -2 4 -9 73.4196 9.63721 1 2 4 9 75.5272 8.79968 1 2 4 9 49.0898 7.86990 2 2 4 9 80.9364 10.6039 7 -2 4 -9 71.1254 9.23110 2 3 -4 9 105.900 11.6938 6 -3 -4 -9 123.106 14.1927 3 -3 -4 -9 100.935 13.2557 8 3 -4 9 106.044 10.3162 7 3 -4 9 108.297 11.9605 1 -3 -4 -9 130.792 12.1317 4 3 -4 9 121.103 12.1737 2 3 4 9 125.183 13.7543 7 3 4 9 130.395 11.0658 6 3 4 9 124.645 10.8224 2 -3 4 -9 119.002 11.7633 3 3 4 9 112.406 10.3539 1 4 -4 9 -5.7253 5.54818 2 -4 -4 -9 1.77846 7.06699 3 4 -4 9 4.61881 5.79677 1 4 -4 9 16.0485 6.91183 6 -4 4 -9 4.39431 8.00483 5 4 4 9 -0.7784 4.14234 1 4 4 9 4.41728 6.42448 7 4 4 9 2.78235 5.04531 6 4 4 9 -9.2229 4.06918 2 -4 4 -9 5.75796 5.99246 3 -5 -4 -9 13.3326 10.4817 5 5 -4 9 9.43954 6.21929 1 5 -4 9 8.70121 6.89364 2 5 -4 9 10.3175 6.90277 6 -5 -4 -9 1.71472 7.46056 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24.9635 8 -9 5 9 75.3197 19.3046 5 9 5 -9 37.2299 13.4919 6 8 -5 -9 20.9678 11.6274 2 8 -5 -9 5.28195 8.63935 1 8 -5 -9 9.25496 17.4979 8 -8 -5 9 24.3190 13.4037 5 8 -5 -9 29.2314 13.4814 6 -8 5 9 2.13844 13.1477 5 8 5 -9 -1.6565 10.7878 6 8 5 -9 -15.292 14.0031 8 8 5 -9 14.3041 9.37739 2 -7 -5 9 111.945 17.9480 5 7 -5 -9 102.296 15.9161 6 7 -5 -9 102.953 21.2988 8 7 -5 -9 126.451 15.9287 2 7 -5 -9 110.127 14.7394 1 7 5 -9 129.169 19.2435 8 7 5 -9 115.529 15.8340 6 7 5 -9 96.7700 12.7568 1 -7 5 9 122.838 18.6602 5 7 5 -9 92.6870 12.7763 2 -7 5 9 135.837 18.8084 3 6 -5 -9 97.6284 13.8888 2 -6 -5 9 84.9534 15.6628 7 -6 -5 9 108.578 17.0387 5 6 -5 -9 104.431 18.6569 8 6 -5 -9 125.510 15.9609 6 6 -5 -9 112.268 14.7384 1 -6 5 9 148.857 17.0165 3 6 5 -9 113.371 16.8838 8 -6 5 9 90.9126 15.5507 5 6 5 -9 109.731 12.9193 1 6 5 -9 102.486 12.7650 2 6 5 -9 132.304 15.0988 6 -6 5 9 112.642 15.0133 7 5 -5 -9 108.841 13.5442 2 -5 -5 9 121.542 16.3246 7 -5 -5 9 106.520 15.4607 5 5 -5 -9 86.2128 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8 3 5 -9 89.8351 11.5570 1 3 5 -9 107.733 11.9807 6 -2 -5 9 115.920 13.3980 5 2 -5 -9 76.4176 10.5363 1 -2 -5 9 93.3055 11.6285 1 -2 -5 9 96.0299 11.3440 2 2 -5 -9 89.3745 13.5334 8 2 -5 -9 111.824 11.7991 2 -2 -5 9 122.421 13.3316 7 -2 5 9 108.773 12.4680 5 2 5 -9 80.8698 11.2282 8 2 5 -9 106.265 11.3658 2 -2 5 9 101.393 10.8594 2 2 5 -9 102.457 11.2589 6 2 5 -9 93.5115 10.9637 1 -2 5 9 101.422 12.0781 7 -2 5 9 91.3930 11.6012 1 -1 -5 9 335.730 17.1221 2 1 -5 -9 332.895 19.9572 8 1 -5 -9 314.433 18.1025 1 -1 -5 9 330.990 17.6768 7 1 -5 -9 293.868 16.1924 4 -1 -5 9 316.732 17.8708 1 1 -5 -9 343.419 17.2438 2 1 5 -9 308.318 17.2667 1 -1 5 9 312.220 16.8825 1 -1 5 9 323.413 16.2313 6 -1 5 9 319.247 17.3025 5 1 5 -9 323.665 16.6109 2 -1 5 9 347.406 16.6930 2 -1 5 9 296.057 17.4221 7 1 5 -9 322.588 19.1358 8 1 5 -9 328.253 18.1047 6 0 -5 9 38.5245 7.58867 2 0 -5 9 49.3224 7.98566 6 0 -5 -9 45.9881 7.83168 2 0 -5 -9 41.0979 7.22852 4 0 -5 -9 47.7868 9.17115 8 0 -5 9 34.2267 7.49478 7 0 -5 9 42.1742 8.31452 1 0 -5 -9 35.5952 7.97247 1 0 5 9 71.8977 10.1581 7 0 5 -9 52.4634 6.28398 3 0 5 -9 49.6593 7.76805 2 0 5 9 52.7698 8.14474 1 0 5 -9 63.3672 9.86726 8 0 5 9 54.1121 7.95661 2 0 5 -9 59.6526 9.34349 1 0 5 9 40.9072 7.24939 6 1 -5 9 850.697 29.6901 2 -1 -5 -9 854.551 29.2723 4 -1 -5 -9 877.814 30.0805 1 1 -5 9 876.338 29.6806 7 -1 -5 -9 881.296 33.1227 8 -1 -5 -9 893.772 31.2441 2 1 -5 9 842.825 29.7093 6 1 -5 9 834.609 30.6308 1 -1 5 -9 830.209 29.4175 2 1 5 9 821.843 28.5286 6 -1 5 -9 877.297 31.0944 1 1 5 9 871.606 28.7936 2 -1 5 -9 830.643 27.0165 3 -1 5 -9 853.227 32.7925 8 1 5 9 820.659 28.9277 1 1 5 9 826.066 30.8036 7 -2 -5 -9 1855.15 55.6175 3 2 -5 9 1876.01 54.6785 1 -2 -5 -9 1817.89 57.2591 8 2 -5 9 1900.88 54.1235 6 2 -5 9 1917.10 52.9306 7 2 -5 9 1867.68 54.0280 2 -2 -5 -9 1830.35 53.3718 4 2 5 9 1861.33 52.1542 1 2 5 9 1871.75 55.8035 7 -2 5 -9 1871.29 53.5515 2 -2 5 -9 1803.44 57.7080 8 -2 5 -9 1845.83 52.5410 3 2 5 9 1894.29 52.4817 6 2 5 9 1906.78 52.1069 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2 -10 162.749 21.5208 5 -7 2 -10 155.615 20.0786 3 7 2 10 185.495 15.2194 6 -8 -2 -10 31.4872 15.3709 5 -8 -2 -10 56.5524 15.0481 3 8 -2 10 63.2047 11.9355 6 -8 2 -10 45.3879 14.5212 3 -8 2 -10 26.5335 15.2606 5 8 2 10 38.2325 9.95827 6 -9 -2 -10 26.8320 14.0306 3 -9 -2 -10 28.1933 17.4893 5 9 -2 10 63.8014 12.7467 6 -9 2 -10 40.1442 17.7060 5 -9 2 -10 23.0345 15.8123 3 9 2 10 43.6880 10.7776 6 9 -3 -10 12.0429 11.5173 2 -9 -3 10 35.6878 16.7684 5 9 -3 -10 22.8560 14.3781 6 9 3 -10 22.6089 11.4878 2 9 3 -10 6.57802 13.2787 6 -9 3 10 31.5606 17.0317 5 8 -3 -10 4.47951 8.93767 1 -8 -3 10 15.2607 12.5392 5 8 -3 -10 20.2578 11.7245 2 8 -3 -10 15.7282 13.0822 6 8 -3 -10 31.6802 19.1096 8 8 3 -10 10.6430 12.3008 6 8 3 -10 4.07364 9.83171 1 8 3 -10 16.1287 16.0313 8 -8 3 10 34.7643 15.4050 5 8 3 -10 3.68517 9.89592 2 7 -3 -10 4.81069 15.5632 8 -7 -3 10 7.29223 11.0772 7 7 -3 -10 16.9787 9.96085 2 7 -3 -10 14.9086 11.2151 6 7 -3 -10 25.4767 10.0748 1 -7 -3 10 28.5352 13.4738 5 7 3 -10 26.8039 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238.172 16.5797 1 -3 4 10 243.549 18.1285 7 3 4 -10 247.153 19.5694 8 -3 4 10 217.882 15.7268 2 -2 -4 10 372.924 20.4823 1 2 -4 -10 392.536 20.0807 2 2 -4 -10 366.414 23.1009 8 -2 -4 10 383.207 21.1606 7 -2 -4 10 393.459 19.9136 2 2 -4 -10 325.928 20.0458 1 -2 -4 10 392.152 22.1577 5 -2 4 10 431.387 20.0362 2 2 4 -10 427.325 20.1948 6 -2 4 10 380.356 20.3093 1 2 4 -10 407.043 23.1761 8 2 4 -10 426.537 20.9745 1 -2 4 10 345.850 20.4884 7 -2 4 10 392.857 20.9025 5 2 4 -10 410.665 20.0665 2 -1 -4 10 698.091 28.5229 1 1 -4 -10 663.158 30.4054 8 1 -4 -10 692.037 26.7181 4 -1 -4 10 714.432 28.4451 7 1 -4 -10 737.571 27.8066 2 -1 -4 10 689.896 27.2278 2 1 -4 -10 668.961 28.0245 1 1 4 -10 730.108 30.2680 8 -1 4 10 685.468 27.6716 1 1 4 -10 660.385 26.7190 2 -1 4 10 731.014 28.7373 5 -1 4 10 693.629 26.7241 2 -1 4 10 706.756 28.5684 7 1 4 -10 686.460 28.0572 1 -1 4 10 718.831 26.9127 6 0 -4 -10 524.562 25.7758 8 0 -4 -10 521.277 22.1344 2 0 -4 10 513.876 23.0398 7 0 -4 -10 492.593 21.5290 4 0 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2 -2 9 18 -25.584 14.4024 5 -1 -9 18 0.09009 17.0955 5 -1 -9 18 33.0689 15.5828 2 1 -9 -18 8.34145 13.4660 4 1 9 -18 4.76179 12.9528 2 -1 9 18 0.05332 11.8511 2 -1 9 18 6.77697 16.5068 5 0 -9 18 20.3359 14.2509 2 0 -9 -18 -12.807 11.5627 4 0 -9 18 -14.715 16.7150 5 0 9 18 -17.649 14.8019 5 0 9 18 12.4565 11.2980 2 1 -9 18 3.77162 14.2163 2 1 9 18 1.70268 11.3230 2 1 9 18 6.42862 18.0251 5 2 -9 18 -1.6238 13.7278 2 2 9 18 -4.2252 10.6425 2 -3 -10 18 42.8590 17.9317 5 3 -10 -18 -2.4277 12.9709 4 -3 10 18 16.6474 14.1132 2 -3 10 18 32.7921 18.1207 5 3 10 -18 34.3343 14.9727 2 -2 -10 18 12.0147 17.1683 5 -2 -10 18 13.4381 15.0033 2 2 -10 -18 2.68474 13.6338 4 -2 10 18 26.3165 14.6123 2 -2 10 18 4.57201 16.8747 5 2 10 -18 33.3065 15.2488 2 -1 -10 18 91.1390 22.8405 5 1 -10 -18 72.9405 17.5388 4 -1 -10 18 80.1823 20.0747 2 -1 10 18 108.130 23.9935 5 -1 10 18 76.0188 17.3089 2 1 10 -18 109.237 21.0582 2 0 -10 -18 36.5127 15.0037 4 0 -10 18 76.0143 21.2776 5 0 -10 18 65.7610 18.1104 2 0 10 18 50.6427 14.3509 2 1 -10 18 131.174 20.4847 2 1 10 18 93.3463 16.7273 2 2 -10 18 49.5808 18.0463 2 2 10 18 126.638 18.4253 2 3 -11 -18 41.2582 16.5477 4 -3 -11 18 26.5845 17.7153 5 3 11 -18 41.9207 15.5446 2 -3 11 18 68.3885 18.4533 2 -2 -11 18 -17.669 14.6109 2 2 -11 -18 3.13297 14.0327 4 -2 -11 18 9.29116 16.9738 5 -2 11 18 16.4370 13.5050 2 2 11 -18 25.3767 14.5893 2 -1 -11 18 -15.984 15.5823 5 -1 -11 18 6.92233 15.4920 2 1 -11 -18 4.23390 13.8268 4 -1 11 18 2.90415 11.9978 2 1 11 -18 8.94727 13.2579 2 0 -11 -18 -2.0563 12.3711 4 0 -11 18 -5.5900 16.3866 5 0 -11 18 2.99507 13.9125 2 0 11 18 14.5498 13.0051 2 1 -11 18 -2.2307 13.3937 2 1 11 18 -0.9549 11.3772 2 2 -12 -18 43.3971 17.7319 4 -2 -12 18 -8.0754 16.4156 5 2 12 -18 23.5444 14.9273 2 -2 12 18 22.7110 13.9310 2 -1 -12 18 74.6064 19.8972 2 -1 -12 18 45.4859 20.7253 5 1 -12 -18 20.5389 15.2976 4 1 12 -18 54.5668 17.3078 2 -1 12 18 51.0250 15.8678 2 0 -12 18 38.0703 16.6246 2 0 -12 -18 29.4271 16.1794 4 0 -12 18 31.3880 19.3409 5 0 12 18 28.8573 13.9119 2 1 -12 18 26.2526 15.7913 2 1 12 18 20.2569 12.6071 2 4 0 -19 13.7974 12.8297 2 -4 0 19 22.1618 19.2232 5 4 0 -19 18.7916 13.4712 4 -3 0 19 4.63950 13.1659 2 3 0 -19 4.09353 12.2663 2 -3 0 19 3.85899 17.5367 5 -2 0 19 13.1338 12.6577 2 -2 0 19 -8.3397 16.1529 5 2 0 -19 -13.351 10.9712 2 -1 0 19 -5.6489 11.5156 2 -1 0 19 -12.506 16.2947 5 0 0 19 13.4228 18.6529 5 0 0 19 -11.110 11.7366 2 1 0 19 4.65365 11.8229 2 2 0 19 -15.551 12.4940 2 -4 -1 19 324.705 35.4240 5 4 -1 -19 358.603 33.2574 2 4 -1 -19 327.647 29.6493 4 -4 1 19 412.223 40.1853 5 4 1 -19 345.821 30.9314 4 4 1 -19 330.467 30.8351 2 -3 -1 19 87.2309 17.8752 2 3 -1 -19 62.5486 16.3599 2 3 -1 -19 68.5233 16.7092 4 -3 -1 19 66.3225 21.2929 5 3 1 -19 96.1378 19.8645 2 -3 1 19 86.5658 18.2661 2 -3 1 19 82.1905 22.0760 5 -2 -1 19 40.6122 15.2531 2 2 -1 -19 25.5654 16.3424 2 -2 -1 19 75.6765 22.6136 5 2 1 -19 75.1680 17.5145 2 -2 1 19 34.5786 20.0749 5 -2 1 19 69.7020 16.5187 2 -1 -1 19 -0.8592 16.6238 5 -1 -1 19 23.5035 14.0734 2 -1 1 19 30.9191 14.0799 2 -1 1 19 13.4292 17.7807 5 0 -1 19 104.637 19.1722 2 0 -1 19 85.5312 22.9441 5 0 1 19 127.044 26.5026 5 0 1 19 89.4990 17.8961 2 1 -1 19 209.584 24.6466 2 1 1 19 167.050 21.5684 2 2 -1 19 135.540 21.2273 2 2 1 19 116.361 19.6349 2 4 -2 -19 -0.8460 12.3121 4 -4 -2 19 9.13491 18.1033 5 4 -2 -19 21.3859 13.6227 2 -4 2 19 6.70000 20.8251 2 -4 2 19 2.70824 18.4971 5 4 2 -19 16.6127 13.9141 2 -3 -2 19 14.9548 16.1471 5 -3 -2 19 -4.5693 12.7034 2 3 -2 -19 20.1678 13.1210 2 3 -2 -19 17.1227 13.0282 4 -3 2 19 35.8245 18.3491 5 3 2 -19 2.81820 12.7753 2 -3 2 19 1.54286 13.8106 2 -2 -2 19 5.99682 17.6390 5 -2 -2 19 13.2691 13.9766 2 2 2 -19 20.9285 13.9040 2 -2 2 19 -11.260 16.7071 5 -2 2 19 -5.5289 12.4165 2 -1 -2 19 85.6564 18.3832 2 -1 -2 19 83.3327 22.9990 5 -1 2 19 20.7773 12.9775 2 -1 2 19 45.3531 20.2342 5 0 -2 19 50.1657 15.6574 2 0 -2 19 62.6536 20.6599 5 0 2 19 61.2119 15.9163 2 0 2 19 62.3556 21.8786 5 1 -2 19 16.9584 13.4988 2 1 2 19 22.3502 13.2137 2 2 -2 19 9.32829 13.4612 2 2 2 19 3.10639 12.7281 2 4 -3 -19 75.4013 17.6819 2 4 -3 -19 111.410 19.6819 4 -4 -3 19 94.0993 23.5890 5 -4 3 19 170.269 28.0083 5 -4 3 19 123.472 21.5218 2 4 3 -19 117.779 20.9028 2 -3 -3 19 195.889 27.9200 5 -3 -3 19 199.608 25.1267 2 3 -3 -19 200.122 24.0761 4 3 -3 -19 163.269 22.4246 2 -3 3 19 252.110 31.8302 5 3 3 -19 181.683 24.0306 2 -3 3 19 208.424 25.8880 2 -2 -3 19 38.3074 19.3289 5 -2 -3 19 78.1996 18.6546 2 -2 3 19 61.7304 16.6267 2 2 3 -19 62.5536 17.4368 2 -2 3 19 32.1893 17.5738 5 -1 -3 19 14.1566 17.9553 5 -1 -3 19 3.59352 12.2054 2 -1 3 19 10.7990 17.9094 5 -1 3 19 25.0542 13.8625 2 0 -3 19 30.0351 18.5443 5 0 -3 19 32.1560 14.5525 2 0 3 19 15.9134 19.1840 5 0 3 19 26.4854 13.4170 2 1 -3 19 13.4207 13.2827 2 1 3 19 55.4163 21.6297 5 1 3 19 8.97651 12.6277 2 2 -3 19 112.087 19.6552 2 2 3 19 60.8910 16.6348 2 -4 -4 19 -1.6247 17.4161 5 4 -4 -19 7.82154 12.6775 4 4 -4 -19 13.6148 14.3713 2 -4 4 19 4.10625 18.5680 5 4 4 -19 16.2489 13.5203 2 -4 4 19 15.2145 15.3252 2 3 -4 -19 25.0777 14.7284 4 3 -4 -19 45.4408 15.6988 2 -3 -4 19 35.3752 17.1449 5 -3 -4 19 67.8932 18.0297 2 3 4 -19 25.1551 14.4358 2 -3 4 19 12.7270 17.7710 5 -3 4 19 30.4554 15.1910 2 2 -4 -19 -2.7983 12.3316 4 -2 -4 19 14.0532 17.0320 5 -2 -4 19 2.32542 13.2053 2 2 4 -19 -5.2869 12.4894 2 -2 4 19 -19.050 15.6654 5 -2 4 19 0.94753 13.3137 2 -1 -4 19 6.06586 17.0525 5 -1 -4 19 5.60029 13.1722 2 -1 4 19 -2.9328 11.7837 2 -1 4 19 26.3113 18.8174 5 0 -4 19 30.4284 14.1936 2 0 -4 19 16.2627 17.0048 5 0 4 19 -3.5537 18.0191 5 0 4 19 15.7129 13.0256 2 1 -4 19 84.3076 18.5389 2 1 4 19 70.8780 15.8919 2 1 4 19 46.7125 21.6627 5 2 -4 19 12.9972 13.5810 2 2 4 19 0.46359 12.8831 2 3 -5 -19 88.5966 18.2060 2 -3 -5 19 46.6319 16.9926 2 3 -5 -19 83.7146 18.9268 4 -3 -5 19 111.929 23.8540 5 -3 5 19 103.085 20.1882 2 -3 5 19 170.084 27.7587 5 3 5 -19 107.321 20.2752 2 2 -5 -19 34.6768 15.3242 4 -2 -5 19 68.8172 21.2953 5 -2 -5 19 25.7631 15.6115 2 -2 5 19 60.6524 21.0126 5 2 5 -19 73.8990 17.9962 2 -2 5 19 39.5696 15.7376 2 -1 -5 19 165.290 27.3287 5 -1 -5 19 179.607 24.0958 2 -1 5 19 216.777 30.1891 5 -1 5 19 166.979 22.7691 2 0 -5 19 85.8010 18.6251 2 0 -5 19 53.6561 21.1679 5 0 5 19 62.4575 15.7738 2 0 5 19 88.7591 23.1985 5 1 -5 19 21.9806 14.6840 2 1 5 19 21.1675 12.4195 2 1 5 19 -12.980 16.2687 5 2 -5 19 66.8744 17.2160 2 2 5 19 33.4790 14.8641 2 3 -6 -19 10.6893 12.3350 2 -3 -6 19 22.1137 17.6927 5 3 -6 -19 4.46015 13.0929 4 3 6 -19 2.41116 12.7092 2 -3 6 19 31.6054 15.5807 2 -3 6 19 22.5724 20.4748 5 -2 -6 19 31.1611 18.7383 5 2 -6 -19 30.2660 14.6122 4 -2 -6 19 25.7235 15.7734 2 2 6 -19 26.2744 14.2647 2 -2 6 19 42.6688 19.3980 5 -2 6 19 14.1069 13.0596 2 -1 -6 19 20.9039 18.8954 5 -1 -6 19 44.2183 15.8644 2 -1 6 19 11.3344 13.0706 2 -1 6 19 3.81369 16.9195 5 0 -6 19 18.2366 18.2073 5 0 -6 19 11.2213 14.7583 2 0 6 19 10.9143 12.3253 2 0 6 19 19.3562 19.0298 5 1 -6 19 10.8910 13.3743 2 1 6 19 3.06525 11.7742 2 1 6 19 36.3214 20.3910 5 2 -6 19 -12.870 12.6626 2 2 6 19 -15.699 10.6384 2 3 -7 -19 41.1916 16.4078 4 -3 -7 19 83.4295 21.0402 5 3 7 -19 80.6109 18.4819 2 -3 7 19 50.0581 16.8025 2 -3 7 19 37.3020 21.7376 5 -2 -7 19 46.7936 19.5001 5 -2 -7 19 61.6907 18.5047 2 2 -7 -19 76.6149 18.8213 4 2 7 -19 89.1892 19.9481 2 -2 7 19 87.0488 18.3351 2 -2 7 19 57.7249 21.0938 5 1 -7 -19 95.5780 20.8994 4 -1 -7 19 111.802 21.2162 2 -1 -7 19 158.038 27.6138 5 -1 7 19 146.130 26.2922 5 -1 7 19 144.580 21.6188 2 0 -7 19 79.2625 19.5206 2 0 -7 19 61.6864 21.1804 5 0 7 19 46.4069 20.6267 5 0 7 19 21.6268 14.2209 2 1 -7 19 63.1893 17.8744 2 1 7 19 13.9768 20.2549 5 1 7 19 45.2756 14.6431 2 -2 -8 19 4.10547 17.9525 5 2 -8 -19 3.35548 14.3194 4 -2 -8 19 5.18559 15.2472 2 -2 8 19 -2.8561 16.8229 5 -2 8 19 3.63223 13.6694 2 2 8 -19 23.1947 14.0853 2 1 -8 -19 -13.274 12.6789 4 -1 -8 19 12.2744 17.1124 2 -1 -8 19 28.9967 18.4531 5 -1 8 19 19.5151 13.0858 2 -1 8 19 17.6474 18.0246 5 1 8 -19 13.7695 15.8566 2 0 -8 19 -23.328 17.0329 5 0 -8 19 -11.428 12.8355 2 0 8 19 -4.6954 11.9072 2 0 8 19 -0.3437 17.4210 5 1 -8 19 17.0513 14.2534 2 1 8 19 -0.0161 18.9303 5 1 8 19 -10.926 10.6327 2 1 -9 -19 89.4705 18.4320 4 -1 -9 19 60.1343 18.6585 2 -1 -9 19 111.308 25.2084 5 1 9 -19 98.1318 19.9734 2 -1 9 19 101.432 19.4508 2 -1 9 19 153.071 24.8809 5 0 -9 19 -1.2703 17.3664 5 0 -9 19 44.4159 17.4183 2 0 9 19 50.9555 14.6868 2 0 9 19 22.4751 18.7585 5 -2 0 20 -3.2460 18.0551 5 -2 0 20 21.6343 13.8443 2 -1 0 20 144.336 22.5500 2 -1 0 20 193.183 30.0725 5 0 0 20 172.837 30.0667 5 0 0 20 225.143 25.8480 2 -2 -1 20 38.7516 21.0654 5 -2 1 20 49.0712 20.9492 5 -1 -1 20 -0.8985 17.6527 5 -1 -1 20 1.89452 12.7385 2 -1 1 20 -0.9016 12.1871 2 -1 1 20 16.8876 19.3512 5 0 -1 20 -5.8477 19.2622 5 0 -1 20 17.4469 13.2912 2 0 1 20 23.0375 19.9590 5 0 1 20 13.6962 13.3033 2 -1 -2 20 42.2733 15.8957 2 -1 -2 20 21.4457 20.2967 5 -1 2 20 15.6112 13.3668 2 -1 2 20 28.1670 20.9378 5 0 -2 20 250.093 33.5436 5 0 -2 20 168.814 23.1262 2 0 2 20 318.948 36.5934 5 0 2 20 238.020 25.6784 2 -1 -3 20 17.2763 18.9562 5 -1 -3 20 33.8566 15.7933 2 -1 3 20 27.4909 20.6334 5 -1 3 20 20.2698 13.6584 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_correction_T_min 0.6334 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 7.097 18.365 12.890 90.023 94.138 89.958 ) ; _shelx_hkl_checksum 10392 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 0.500000 0.500000 0.500000 0.01356(7) Uani 1 2 d S . P . . O1 O 0.40734(18) 0.58917(7) 0.45986(9) 0.0156(2) Uani 1 1 d . . . . . O2 O 0.42246(18) 0.46357(7) 0.37182(9) 0.0143(2) Uani 1 1 d . . . . . O3 O 0.76621(19) 0.53043(7) 0.45013(10) 0.0178(2) Uani 1 1 d . . . . . C1 C 0.3616(2) 0.58827(9) 0.35505(12) 0.0129(3) Uani 1 1 d . . . . . C2 C 0.3655(2) 0.52001(9) 0.30728(13) 0.0131(3) Uani 1 1 d . . . . . C3 C 0.3187(2) 0.51243(9) 0.20005(13) 0.0137(3) Uani 1 1 d . . . . . C4 C 0.2787(2) 0.57729(10) 0.14440(13) 0.0146(3) Uani 1 1 d . . . . . H4 H 0.247157 0.573910 0.071664 0.018 Uiso 1 1 calc R U . . . C5 C 0.2828(2) 0.64635(10) 0.19015(13) 0.0143(3) Uani 1 1 d . . . . . C6 C 0.3233(2) 0.65111(10) 0.29830(13) 0.0147(3) Uani 1 1 d . . . . . H6 H 0.324339 0.697124 0.332090 0.018 Uiso 1 1 calc R U . . . C7 C 0.3121(2) 0.43693(9) 0.14742(12) 0.0136(3) Uani 1 1 d . . . . . C8 C 0.2602(3) 0.44171(11) 0.03027(14) 0.0194(3) Uani 1 1 d . . . . . H8A H 0.355053 0.470929 -0.002548 0.029 Uiso 1 1 calc R U . . . H8B H 0.135753 0.464654 0.018015 0.029 Uiso 1 1 calc R U . . . H8C H 0.256425 0.392604 0.000343 0.029 Uiso 1 1 calc R U . . . C9 C 0.1597(3) 0.39078(11) 0.19634(15) 0.0245(4) Uani 1 1 d . . . . . H9A H 0.158095 0.341658 0.166492 0.037 Uiso 1 1 calc R U . . . H9B H 0.035614 0.413577 0.181881 0.037 Uiso 1 1 calc R U . . . H9C H 0.188607 0.387786 0.271727 0.037 Uiso 1 1 calc R U . . . C10 C 0.5029(3) 0.39878(11) 0.16425(15) 0.0220(4) Uani 1 1 d . . . . . H10A H 0.495382 0.350538 0.131627 0.033 Uiso 1 1 calc R U . . . H10B H 0.536097 0.393446 0.238995 0.033 Uiso 1 1 calc R U . . . H10C H 0.599913 0.427839 0.132933 0.033 Uiso 1 1 calc R U . . . C11 C 0.2584(3) 0.71671(10) 0.12647(14) 0.0175(3) Uani 1 1 d . . . . . C12 C 0.1391(3) 0.77284(12) 0.18134(17) 0.0280(4) Uani 1 1 d . . . . . H12A H 0.132055 0.818152 0.141030 0.042 Uiso 1 1 calc R U . . . H12B H 0.197746 0.782606 0.251129 0.042 Uiso 1 1 calc R U . . . H12C H 0.011318 0.753536 0.186840 0.042 Uiso 1 1 calc R U . . . C13 C 0.1605(3) 0.70356(12) 0.01840(16) 0.0280(4) Uani 1 1 d . . . . . H13A H 0.238177 0.670909 -0.021008 0.042 Uiso 1 1 calc R U . . . H13B H 0.144195 0.750097 -0.018422 0.042 Uiso 1 1 calc R U . . . H13C H 0.036549 0.681241 0.025398 0.042 Uiso 1 1 calc R U . . . C14 C 0.4548(3) 0.74878(12) 0.11336(17) 0.0267(4) Uani 1 1 d . . . . . H14A H 0.528295 0.714677 0.073899 0.040 Uiso 1 1 calc R U . . . H14B H 0.519995 0.757041 0.181998 0.040 Uiso 1 1 calc R U . . . H14C H 0.441681 0.795137 0.075807 0.040 Uiso 1 1 calc R U . . . C15 C 0.8407(3) 0.50790(11) 0.35253(15) 0.0219(4) Uani 1 1 d . . . . . H15A H 0.765066 0.467400 0.320390 0.026 Uiso 1 1 calc R U . . . H15B H 0.973921 0.491937 0.364117 0.026 Uiso 1 1 calc R U . . . C16 C 0.8257(3) 0.57545(12) 0.28379(15) 0.0239(4) Uani 1 1 d . . . . . H16A H 0.706688 0.574966 0.238632 0.029 Uiso 1 1 calc R U . . . H16B H 0.933785 0.578404 0.239460 0.029 Uiso 1 1 calc R U . . . C17 C 0.8283(3) 0.63978(12) 0.36087(16) 0.0235(4) Uani 1 1 d . . . . . H17A H 0.939783 0.671284 0.353175 0.028 Uiso 1 1 calc R U . . . H17B H 0.712289 0.669568 0.349414 0.028 Uiso 1 1 calc R U . . . C18 C 0.8383(3) 0.60435(11) 0.46766(15) 0.0227(4) Uani 1 1 d . . . . . H18A H 0.970229 0.603256 0.498476 0.027 Uiso 1 1 calc R U . . . H18B H 0.759433 0.631337 0.515035 0.027 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 Ge1 0.01856(12) 0.01370(12) 0.00837(10) 0.00010(9) 0.00067(8) -0.00022(10) O1 0.0228(6) 0.0150(6) 0.0089(5) 0.0005(4) 0.0001(4) 0.0018(5) O2 0.0211(6) 0.0137(6) 0.0081(5) 0.0004(4) 0.0003(4) -0.0001(4) O3 0.0210(6) 0.0190(6) 0.0141(6) -0.0014(5) 0.0050(5) -0.0035(5) C1 0.0136(7) 0.0170(8) 0.0082(6) 0.0002(5) 0.0009(5) 0.0002(6) C2 0.0145(7) 0.0146(7) 0.0105(6) 0.0016(5) 0.0023(5) -0.0004(5) C3 0.0134(7) 0.0159(8) 0.0120(7) 0.0005(5) 0.0019(5) -0.0001(5) C4 0.0154(7) 0.0174(8) 0.0111(7) 0.0010(6) 0.0006(5) 0.0014(6) C5 0.0141(7) 0.0165(7) 0.0125(7) 0.0021(6) 0.0021(5) 0.0008(6) C6 0.0167(7) 0.0150(7) 0.0125(7) 0.0006(6) 0.0013(6) 0.0010(6) C7 0.0183(7) 0.0127(7) 0.0099(6) -0.0003(5) 0.0008(5) -0.0013(6) C8 0.0236(8) 0.0213(9) 0.0133(7) -0.0020(6) 0.0011(6) -0.0001(7) C9 0.0331(10) 0.0236(9) 0.0176(8) -0.0034(7) 0.0066(7) -0.0100(8) C10 0.0277(9) 0.0218(9) 0.0163(8) -0.0028(7) 0.0010(7) 0.0073(7) C11 0.0225(8) 0.0155(8) 0.0146(7) 0.0033(6) 0.0020(6) 0.0030(6) C12 0.0385(11) 0.0226(10) 0.0233(9) 0.0030(8) 0.0051(8) 0.0114(8) C13 0.0395(12) 0.0250(10) 0.0183(9) 0.0042(7) -0.0064(8) 0.0028(9) C14 0.0308(10) 0.0223(10) 0.0274(10) 0.0082(8) 0.0043(8) -0.0032(8) C15 0.0206(8) 0.0272(10) 0.0187(8) -0.0039(7) 0.0071(6) 0.0004(7) C16 0.0191(8) 0.0368(11) 0.0163(8) 0.0031(7) 0.0038(6) -0.0039(8) C17 0.0203(8) 0.0242(9) 0.0260(9) 0.0066(8) 0.0016(7) -0.0034(7) C18 0.0259(9) 0.0225(9) 0.0199(8) -0.0016(7) 0.0034(7) -0.0071(7) 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' O O 0.0106 0.0060 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 O1 180.0 3_666 . ? O1 Ge1 O2 89.60(6) 3_666 3_666 ? O1 Ge1 O2 90.40(6) . 3_666 ? O1 Ge1 O2 90.40(6) 3_666 . ? O1 Ge1 O2 89.60(6) . . ? O2 Ge1 O2 180.0 3_666 . ? O1 Ge1 O3 89.31(6) 3_666 3_666 ? O1 Ge1 O3 90.69(6) . 3_666 ? O2 Ge1 O3 92.23(6) 3_666 3_666 ? O2 Ge1 O3 87.77(6) . 3_666 ? O1 Ge1 O3 90.69(6) 3_666 . ? O1 Ge1 O3 89.31(6) . . ? O2 Ge1 O3 87.77(6) 3_666 . ? O2 Ge1 O3 92.23(6) . . ? O3 Ge1 O3 180.0 3_666 . ? C1 O1 Ge1 108.93(11) . . ? C2 O2 Ge1 109.15(11) . . ? C15 O3 C18 104.60(14) . . ? C15 O3 Ge1 125.06(11) . . ? C18 O3 Ge1 120.57(11) . . ? O1 C1 C6 122.46(15) . . ? O1 C1 C2 115.83(15) . . ? C6 C1 C2 121.63(15) . . ? O2 C2 C1 115.11(15) . . ? O2 C2 C3 124.09(16) . . ? C1 C2 C3 120.77(15) . . ? C2 C3 C4 116.23(15) . . ? C2 C3 C7 121.29(15) . . ? C4 C3 C7 122.48(15) . . ? C5 C4 C3 123.69(15) . . ? C5 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? C4 C5 C6 118.13(16) . . ? C4 C5 C11 122.69(15) . . ? C6 C5 C11 119.04(16) . . ? C1 C6 C5 119.42(16) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C10 C7 C8 108.33(14) . . ? C10 C7 C3 110.57(14) . . ? C8 C7 C3 112.33(14) . . ? C10 C7 C9 109.27(16) . . ? C8 C7 C9 107.99(15) . . ? C3 C7 C9 108.28(14) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 108.46(17) . . ? C13 C11 C5 112.37(16) . . ? C14 C11 C5 108.33(15) . . ? C13 C11 C12 107.21(17) . . ? C14 C11 C12 109.15(17) . . ? C5 C11 C12 111.26(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 104.85(16) . . ? O3 C15 H15A 110.8 . . ? C16 C15 H15A 110.8 . . ? O3 C15 H15B 110.8 . . ? C16 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C15 C16 C17 104.56(16) . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? C18 C17 C16 104.67(17) . . ? C18 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? C18 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? O3 C18 C17 105.34(15) . . ? O3 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? O3 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.8247(13) 3_666 ? Ge1 O1 1.8247(13) . ? Ge1 O2 1.8297(13) 3_666 ? Ge1 O2 1.8298(13) . ? Ge1 O3 2.1126(14) 3_666 ? Ge1 O3 2.1126(14) . ? O1 C1 1.366(2) . ? O2 C2 1.371(2) . ? O3 C15 1.459(2) . ? O3 C18 1.462(2) . ? C1 C6 1.382(2) . ? C1 C2 1.397(2) . ? C2 C3 1.405(2) . ? C3 C4 1.408(2) . ? C3 C7 1.542(2) . ? C4 C5 1.397(2) . ? C4 H4 0.9500 . ? C5 C6 1.405(2) . ? C5 C11 1.533(2) . ? C6 H6 0.9500 . ? C7 C10 1.525(3) . ? C7 C8 1.531(2) . ? C7 C9 1.543(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.530(3) . ? C11 C14 1.532(3) . ? C11 C12 1.538(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.523(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.542(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.519(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C15 H15A O2 0.99 2.56 3.103(2) 114.0 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ge1 O1 C1 169.25(11) 3_666 . . . ? O2 Ge1 O1 C1 -10.75(11) . . . . ? O3 Ge1 O1 C1 -98.52(11) 3_666 . . . ? O3 Ge1 O1 C1 81.48(11) . . . . ? O1 Ge1 O2 C2 -170.55(11) 3_666 . . . ? O1 Ge1 O2 C2 9.45(11) . . . . ? O3 Ge1 O2 C2 100.16(11) 3_666 . . . ? O3 Ge1 O2 C2 -79.84(11) . . . . ? Ge1 O1 C1 C6 -166.94(13) . . . . ? Ge1 O1 C1 C2 9.83(18) . . . . ? Ge1 O2 C2 C1 -6.04(18) . . . . ? Ge1 O2 C2 C3 172.12(13) . . . . ? O1 C1 C2 O2 -2.6(2) . . . . ? C6 C1 C2 O2 174.22(15) . . . . ? O1 C1 C2 C3 179.20(15) . . . . ? C6 C1 C2 C3 -4.0(3) . . . . ? O2 C2 C3 C4 -174.78(15) . . . . ? C1 C2 C3 C4 3.3(2) . . . . ? O2 C2 C3 C7 5.3(3) . . . . ? C1 C2 C3 C7 -176.69(15) . . . . ? C2 C3 C4 C5 -0.3(2) . . . . ? C7 C3 C4 C5 179.68(16) . . . . ? C3 C4 C5 C6 -2.1(3) . . . . ? C3 C4 C5 C11 173.63(16) . . . . ? O1 C1 C6 C5 178.10(15) . . . . ? C2 C1 C6 C5 1.5(3) . . . . ? C4 C5 C6 C1 1.4(2) . . . . ? C11 C5 C6 C1 -174.42(15) . . . . ? C2 C3 C7 C10 -58.2(2) . . . . ? C4 C3 C7 C10 121.79(17) . . . . ? C2 C3 C7 C8 -179.39(15) . . . . ? C4 C3 C7 C8 0.6(2) . . . . ? C2 C3 C7 C9 61.4(2) . . . . ? C4 C3 C7 C9 -118.53(18) . . . . ? C4 C5 C11 C13 20.9(2) . . . . ? C6 C5 C11 C13 -163.43(17) . . . . ? C4 C5 C11 C14 -98.9(2) . . . . ? C6 C5 C11 C14 76.8(2) . . . . ? C4 C5 C11 C12 141.14(18) . . . . ? C6 C5 C11 C12 -43.2(2) . . . . ? C18 O3 C15 C16 -39.55(18) . . . . ? Ge1 O3 C15 C16 106.02(15) . . . . ? O3 C15 C16 C17 24.91(19) . . . . ? C15 C16 C17 C18 -1.75(19) . . . . ? C15 O3 C18 C17 38.50(19) . . . . ? Ge1 O3 C18 C17 -108.98(14) . . . . ? C16 C17 C18 O3 -22.0(2) . . . . ?