#------------------------------------------------------------------------------ #$Date: 2024-10-06 10:06:31 +0300 (Sun, 06 Oct 2024) $ #$Revision: 295190 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572143.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_1572143 loop_ _publ_author_name 'Kreimer, Lisa N.' 'Hadlington, Terrance J.' _publ_section_title ; Macrocyclic bis-diphosphenes demonstrating bimetallic exo- and endo-cyclic binding modes. ; _journal_issue 35 _journal_name_full 'Chemical science' _journal_page_first 14154 _journal_page_last 14160 _journal_paper_doi 10.1039/d4sc03516j _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C50 H78 Cl2 Ge N6 O1.50 P2' _chemical_formula_sum 'C50 H78 Cl2 Ge N6 O1.5 P2' _chemical_formula_weight 992.61 _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-05-23 deposited with the CCDC. 2024-07-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.370(4) _cell_length_b 18.920(4) _cell_length_c 33.750(7) _cell_measurement_reflns_used 2000 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 32.50 _cell_measurement_theta_min 1.92 _cell_volume 11092(4) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_detector Pilatus300K _diffrn_detector_area_resol_mean 5.81 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'STOE StadiVari' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation '0.6 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_unetI/netI 0.0886 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 36330 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 2.525 _diffrn_source 'Genix 3D HF Mo' _diffrn_source_current 1.000 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'STOE X-AREA 1.76' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.189 _exptl_crystal_description rod _exptl_crystal_F_000 4224 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 1.225 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 556 _refine_ls_number_reflns 10849 _refine_ls_number_restraints 17 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.1609 _refine_ls_R_factor_gt 0.0792 _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^)+(0.1470P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2137 _refine_ls_wR_factor_ref 0.2622 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5428 _reflns_number_total 10849 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03516j2.cif _cod_data_source_block 1b_GeCl2 _cod_depositor_comments 'Adding full bibliography for 1572143--1572150.cif.' _cod_original_formula_sum 'C50 H78 Cl2 Ge N6 O1.50 P2' _cod_database_code 1572143 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; REM Old TITL Pccn in Pccn REM SHELXT solution in Pccn: R1 0.221, Rweak 0.022, Alpha 0.053 REM 0.340 for 895 systematic absences, Orientation as input REM Formula found by SHELXT: C93 N10 O4 P2 Cl6 Ge2 REM C:\XRay\TH153_~1\Pccn_a.res in Pccn REM wR2 = 0.2578, GooF = S = 1.023, Restrained GooF = 1.023 for all data REM R1 = 0.0796 for 5428 Fo > 4sig(Fo) and 0.1615 for all 10849 data REM 525 parameters refined using 0 restraints REM Highest difference peak 1.114, deepest hole -0.570, 1-sigma level 0.085 REM C:\XRay\TH153_~1\Pccn_a.res in Pccn REM wR2 = 0.2608, GooF = S = 0.999, Restrained GooF = 1.000 for all data REM R1 = 0.0795 for 5428 Fo > 4sig(Fo) and 0.1613 for all 10849 data REM 526 parameters refined using 2 restraints REM Highest difference peak 1.177, deepest hole -0.590, 1-sigma level 0.088 TITL C:\XRay\TH153_~1\Pccn_a.res in Pccn C:\XRay\TH153_~1\Pccn_a.res created by SHELXL-2018/3 at 16:29:02 on 17-May-2024 CELL 0.71073 17.3700 18.9200 33.7500 90.000 90.000 90.000 ZERR 8.0000 0.0035 0.0038 0.0067 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, Z SYMM 0.5+X, -Y, 0.5-Z SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P CL GE UNIT 400 624 48 12 16 16 8 MERG 2 OMIT -2 52 FMAP GRID PLAN TEMP -123 BOND DANG 2.50 0.005 N6 C50 DFIX 1.10 0.005 N6 C49 DFIX 1.52 0.005 C42 C43 C44 C45 C45 C46 DFIX 1.52 0.005 C16 C17A C16 C18A C16 C19A DFIX 1.52 0.005 C20 C21A C20 C22A C20 C23A DFIX 1.52 0.005 C16 C17 C16 C18 C16 C19 DFIX 1.52 0.005 C20 C21 C20 C22 C20 C23 L.S. 20 ACTA WGHT 0.147000 FVAR 0.13807 0.84348 GE1 7 0.460728 0.530291 0.604293 11.00000 0.04925 0.05100 = 0.05733 0.00043 -0.00372 -0.01070 CL2 6 0.373126 0.133251 0.501347 11.00000 0.04662 0.04214 = 0.05486 -0.00142 0.00361 -0.00018 P03 5 0.568028 0.582063 0.641994 11.00000 0.03805 0.04613 = 0.05063 -0.00282 0.00292 -0.00329 P004 5 0.447190 0.419855 0.642317 11.00000 0.04340 0.04714 = 0.05522 -0.00417 -0.00197 -0.00448 CL1 6 0.541040 0.477734 0.558674 11.00000 0.09084 0.08235 = 0.05902 -0.01534 0.01727 -0.02434 O1 4 0.453264 0.538770 0.690266 11.00000 0.03515 0.04741 = 0.05502 -0.00397 0.00589 -0.00494 N3 3 0.326154 0.387578 0.584783 11.00000 0.05203 0.04231 = 0.05823 -0.00292 -0.01106 -0.00615 N4 3 0.415143 0.307768 0.590779 11.00000 0.05031 0.04467 = 0.06374 -0.00442 -0.00275 -0.00387 N1 3 0.575927 0.685791 0.577760 11.00000 0.04700 0.04900 = 0.05258 0.00012 0.00373 -0.00149 N2 3 0.682189 0.628069 0.589465 11.00000 0.04486 0.05257 = 0.06048 -0.00010 0.01298 -0.00372 C1 1 0.457865 0.610994 0.696414 11.00000 0.03518 0.04512 = 0.05053 -0.00460 -0.00370 -0.00297 C2 1 0.513685 0.644848 0.673101 11.00000 0.03421 0.05209 = 0.05134 -0.00456 -0.00213 0.00010 C3 1 0.525883 0.716379 0.679911 11.00000 0.04130 0.05310 = 0.05270 -0.00023 -0.00719 -0.00411 AFIX 43 H3 2 0.563845 0.740779 0.664962 11.00000 -1.20000 AFIX 0 C24 1 0.606854 0.637612 0.602343 11.00000 0.03545 0.05408 = 0.05257 -0.00825 0.00047 -0.00656 C4 1 0.482089 0.754076 0.709165 11.00000 0.03967 0.04666 = 0.06922 -0.00837 -0.00846 0.00031 C33 1 0.392525 0.370655 0.604681 11.00000 0.04717 0.05013 = 0.05776 -0.00138 0.00038 -0.00454 C13 1 0.384358 0.505872 0.698934 11.00000 0.03518 0.05056 = 0.05246 0.00400 -0.00305 -0.00508 C6 1 0.411737 0.645111 0.723957 11.00000 0.03628 0.05804 = 0.04918 -0.00537 0.00169 0.00267 C12 1 0.370662 0.445407 0.677142 11.00000 0.04373 0.04849 = 0.05219 0.00839 -0.00301 -0.00243 C8 1 0.333869 0.534745 0.726833 11.00000 0.03681 0.06502 = 0.05127 0.00002 0.00041 -0.00492 C11 1 0.303507 0.406291 0.687078 11.00000 0.04998 0.06019 = 0.05643 0.01712 -0.00418 -0.01320 AFIX 43 H11 2 0.293537 0.362983 0.673790 11.00000 -1.20000 AFIX 0 C7 1 0.353793 0.602809 0.748538 11.00000 0.03835 0.06774 = 0.05241 -0.00291 0.00598 0.00166 C5 1 0.427210 0.716377 0.729808 11.00000 0.04558 0.05593 = 0.06372 -0.01475 -0.00199 0.01134 AFIX 43 H5 2 0.398074 0.740767 0.749315 11.00000 -1.20000 AFIX 0 C9 1 0.267959 0.493899 0.733999 11.00000 0.04031 0.08042 = 0.06208 0.01439 0.00559 0.00294 AFIX 43 H9 2 0.231607 0.511239 0.752648 11.00000 -1.20000 AFIX 0 C36 1 0.281616 0.454105 0.586716 11.00000 0.05483 0.04705 = 0.06358 0.00140 -0.01094 -0.00859 AFIX 13 H36 2 0.305330 0.485087 0.607387 11.00000 -1.20000 AFIX 0 C10 1 0.252256 0.429703 0.715629 11.00000 0.04034 0.07452 = 0.05989 0.01340 -0.00582 -0.01513 C27 1 0.739851 0.579869 0.606307 11.00000 0.04315 0.06255 = 0.06899 0.00372 0.01007 0.00386 AFIX 13 H27 2 0.717759 0.557856 0.630728 11.00000 -1.20000 AFIX 0 C39 1 0.486399 0.268120 0.602556 11.00000 0.05078 0.05745 = 0.06685 0.00223 -0.00286 0.00012 AFIX 13 H39 2 0.510118 0.292793 0.625742 11.00000 -1.20000 AFIX 0 C34 1 0.309628 0.334224 0.558497 11.00000 0.06042 0.05454 = 0.06493 -0.00766 -0.01479 -0.00312 AFIX 43 H34 2 0.266930 0.332715 0.540927 11.00000 -1.20000 AFIX 0 C37 1 0.286261 0.492149 0.547086 11.00000 0.06967 0.06673 = 0.07312 0.01006 -0.02068 -0.00834 AFIX 137 H37A 2 0.340373 0.498634 0.539715 11.00000 -1.50000 H37B 2 0.261192 0.538391 0.549251 11.00000 -1.50000 H37C 2 0.260211 0.463935 0.526758 11.00000 -1.50000 AFIX 0 C16 1 0.499569 0.832848 0.717297 11.00000 0.04672 0.05537 = 0.07758 -0.01296 -0.00224 0.00556 PART 1 C21 1 0.203346 0.353952 0.769316 21.00000 0.04244 0.07067 = 0.09438 0.02423 0.01040 -0.01365 AFIX 137 H21A 2 0.158473 0.329240 0.780172 21.00000 -1.50000 H21B 2 0.219152 0.391498 0.787590 21.00000 -1.50000 H21C 2 0.245793 0.320382 0.765887 21.00000 -1.50000 PART 0 AFIX 0 C35 1 0.364767 0.284329 0.562042 11.00000 0.06883 0.06043 = 0.07062 -0.01725 -0.01084 -0.01056 AFIX 43 H35 2 0.368207 0.241396 0.547553 11.00000 -1.20000 AFIX 0 C32 1 0.488376 0.788083 0.579182 11.00000 0.06759 0.06416 = 0.10240 0.01770 0.01549 0.01467 AFIX 137 H32A 2 0.515976 0.804483 0.602780 11.00000 -1.50000 H32B 2 0.434259 0.802402 0.580911 11.00000 -1.50000 H32C 2 0.511690 0.808996 0.555482 11.00000 -1.50000 AFIX 0 C30 1 0.493317 0.708395 0.576674 11.00000 0.04837 0.06379 = 0.07279 0.00971 -0.00121 0.00025 AFIX 13 H30 2 0.465942 0.687486 0.599955 11.00000 -1.20000 AFIX 0 C38 1 0.198468 0.439131 0.598670 11.00000 0.05824 0.07514 = 0.07303 0.00077 -0.00794 0.00548 AFIX 137 H38A 2 0.172382 0.413728 0.577220 11.00000 -1.50000 H38B 2 0.171779 0.483869 0.603719 11.00000 -1.50000 H38C 2 0.197849 0.410182 0.622746 11.00000 -1.50000 AFIX 0 C14 1 0.280853 0.646502 0.756576 11.00000 0.04630 0.07409 = 0.08597 -0.00498 0.01334 0.01074 AFIX 137 H14A 2 0.257081 0.659927 0.731340 11.00000 -1.50000 H14B 2 0.294559 0.689192 0.771430 11.00000 -1.50000 H14C 2 0.244409 0.618247 0.772082 11.00000 -1.50000 AFIX 0 C25 1 0.694524 0.670121 0.557014 11.00000 0.06015 0.05465 = 0.06700 0.00530 0.01528 -0.00626 AFIX 43 H25 2 0.740910 0.673233 0.542204 11.00000 -1.20000 AFIX 0 C26 1 0.628384 0.706684 0.549771 11.00000 0.07123 0.05934 = 0.06173 0.00568 0.01818 -0.00248 AFIX 43 H26 2 0.620211 0.740227 0.529252 11.00000 -1.20000 AFIX 0 C15 1 0.390565 0.582762 0.788746 11.00000 0.05936 0.07745 = 0.05390 -0.00512 -0.00181 -0.00594 AFIX 137 H15A 2 0.352544 0.558024 0.805115 11.00000 -1.50000 H15B 2 0.407504 0.625738 0.802411 11.00000 -1.50000 H15C 2 0.434939 0.551826 0.784184 11.00000 -1.50000 AFIX 0 C29 1 0.758787 0.522462 0.577652 11.00000 0.06585 0.06172 = 0.09336 -0.00241 0.00772 0.01155 AFIX 137 H29A 2 0.711495 0.497677 0.570056 11.00000 -1.50000 H29B 2 0.794509 0.489012 0.590042 11.00000 -1.50000 H29C 2 0.782802 0.542966 0.554024 11.00000 -1.50000 AFIX 0 C20 1 0.182574 0.386148 0.729407 11.00000 0.05857 0.08381 = 0.08404 0.03039 0.00178 -0.02138 O2 4 0.250000 0.750000 0.609769 10.50000 0.17268 C28 1 0.810635 0.624155 0.618306 11.00000 0.04948 0.08922 = 0.09530 -0.00571 0.00269 0.00445 AFIX 137 H28A 2 0.832748 0.646485 0.594707 11.00000 -1.50000 H28B 2 0.849181 0.593376 0.630630 11.00000 -1.50000 H28C 2 0.794962 0.660748 0.637207 11.00000 -1.50000 AFIX 0 C31 1 0.455830 0.680643 0.538399 11.00000 0.08716 0.11742 = 0.09161 0.01474 -0.03557 -0.01540 AFIX 137 H31A 2 0.477200 0.705919 0.515565 11.00000 -1.50000 H31B 2 0.400086 0.688357 0.539572 11.00000 -1.50000 H31C 2 0.466331 0.629982 0.535687 11.00000 -1.50000 PART 1 AFIX 0 C19 1 0.459475 0.861565 0.754111 21.00000 0.07138 0.07709 = 0.13236 -0.05153 0.02363 -0.01560 AFIX 137 H19A 2 0.477613 0.909689 0.759423 21.00000 -1.50000 H19B 2 0.471331 0.831232 0.776843 21.00000 -1.50000 H19C 2 0.403705 0.862236 0.749734 21.00000 -1.50000 PART 0 AFIX 0 C40 1 0.466445 0.195346 0.614741 11.00000 0.08655 0.08387 = 0.18266 0.06036 0.00427 0.01020 AFIX 137 H40A 2 0.432448 0.197004 0.637896 11.00000 -1.50000 H40B 2 0.513556 0.169527 0.621506 11.00000 -1.50000 H40C 2 0.440103 0.171262 0.592900 11.00000 -1.50000 AFIX 0 C48 1 0.516822 1.005496 0.589958 11.00000 0.11335 C41 1 0.543106 0.268861 0.569161 11.00000 0.08617 0.17499 = 0.11047 0.02606 0.02040 0.04015 AFIX 137 H41A 2 0.589870 0.243643 0.577164 11.00000 -1.50000 H41B 2 0.556072 0.317842 0.562479 11.00000 -1.50000 H41C 2 0.520502 0.245581 0.545977 11.00000 -1.50000 AFIX 0 C47 1 0.490471 0.989605 0.553052 11.00000 0.11705 AFIX 137 H47A 2 0.447520 0.956222 0.555119 11.00000 -1.50000 H47B 2 0.532053 0.968237 0.537506 11.00000 -1.50000 H47C 2 0.472862 1.032909 0.539949 11.00000 -1.50000 PART 1 AFIX 0 C18 1 0.585313 0.843409 0.725348 21.00000 0.06248 0.06362 = 0.10941 -0.02402 0.00058 -0.00736 AFIX 137 H18A 2 0.596813 0.894083 0.726415 21.00000 -1.50000 H18B 2 0.615348 0.821441 0.704075 21.00000 -1.50000 H18C 2 0.598805 0.821481 0.750722 21.00000 -1.50000 PART 0 AFIX 0 C46 1 0.716283 0.231434 0.515809 11.00000 0.11473 AFIX 23 H46A 2 0.684463 0.248253 0.493373 11.00000 -1.20000 H46B 2 0.688098 0.242696 0.540510 11.00000 -1.20000 PART 1 AFIX 0 C17 1 0.476896 0.878693 0.682078 21.00000 0.20002 0.04079 = 0.12649 -0.00721 -0.07425 0.01436 AFIX 137 H17A 2 0.423341 0.868871 0.674789 21.00000 -1.50000 H17B 2 0.510593 0.868037 0.659568 21.00000 -1.50000 H17C 2 0.482165 0.928666 0.689219 21.00000 -1.50000 PART 0 AFIX 0 C43 1 0.236010 0.632164 0.633591 11.00000 0.15100 AFIX 137 H43A 2 0.209918 0.643830 0.658492 11.00000 -1.50000 H43B 2 0.262974 0.586952 0.636445 11.00000 -1.50000 H43C 2 0.197918 0.628514 0.612269 11.00000 -1.50000 AFIX 0 N5 3 0.535716 1.019783 0.619839 11.00000 0.18358 PART 1 C23 1 0.172175 0.322113 0.702575 21.00000 0.13545 0.23495 = 0.10192 0.00838 0.01640 -0.13797 AFIX 137 H23A 2 0.130273 0.292563 0.712756 21.00000 -1.50000 H23B 2 0.219978 0.294619 0.702006 21.00000 -1.50000 H23C 2 0.159586 0.337960 0.675700 21.00000 -1.50000 AFIX 0 C22 1 0.109584 0.430772 0.730129 21.00000 0.02037 0.17645 = 0.39509 0.19043 0.00125 -0.00342 AFIX 137 H22A 2 0.097691 0.446914 0.703225 21.00000 -1.50000 H22B 2 0.117387 0.471794 0.747397 21.00000 -1.50000 H22C 2 0.066721 0.402315 0.740229 21.00000 -1.50000 PART 0 AFIX 0 C42 1 0.293271 0.689391 0.623694 11.00000 0.29423 AFIX 23 H42A 2 0.323583 0.702136 0.647485 11.00000 -1.20000 H42B 2 0.329164 0.672879 0.602873 11.00000 -1.20000 AFIX 0 C45 1 0.723535 0.152258 0.512727 11.00000 0.24622 AFIX 23 H45A 2 0.755381 0.133960 0.534786 11.00000 -1.20000 H45B 2 0.748699 0.139309 0.487428 11.00000 -1.20000 AFIX 0 C44 1 0.643038 0.120280 0.514600 11.00000 0.30024 AFIX 137 H44A 2 0.604573 0.157943 0.512265 11.00000 -1.50000 H44B 2 0.636316 0.095749 0.539939 11.00000 -1.50000 H44C 2 0.636489 0.086597 0.492801 11.00000 -1.50000 AFIX 0 C49 1 0.681518 0.305327 0.646440 11.00000 0.25241 N6 3 0.645992 0.265585 0.662160 11.00000 0.23207 C50 1 0.683010 0.386782 0.640477 11.00000 0.24427 AFIX 137 H50A 2 0.652967 0.399168 0.616900 11.00000 -1.50000 H50B 2 0.736322 0.402566 0.637010 11.00000 -1.50000 H50C 2 0.660682 0.409966 0.663762 11.00000 -1.50000 PART 2 AFIX 0 C17A 1 0.424315 0.861614 0.700736 -21.00000 0.11634 AFIX 137 H17D 2 0.380949 0.840549 0.715074 -21.00000 -1.50000 H17E 2 0.420444 0.849725 0.672544 -21.00000 -1.50000 H17F 2 0.423104 0.913085 0.703928 -21.00000 -1.50000 AFIX 0 C18A 1 0.570637 0.859200 0.695570 -21.00000 0.04810 AFIX 137 H18D 2 0.565180 0.909813 0.690071 -21.00000 -1.50000 H18E 2 0.576278 0.833397 0.670560 -21.00000 -1.50000 H18F 2 0.616275 0.851382 0.712069 -21.00000 -1.50000 AFIX 0 C19A 1 0.498330 0.843367 0.761953 -21.00000 0.11091 AFIX 31 H19D 2 0.546344 0.825398 0.773400 -21.00000 -1.50000 H19E 2 0.454599 0.817649 0.773299 -21.00000 -1.50000 H19F 2 0.493247 0.893834 0.767944 -21.00000 -1.50000 AFIX 0 C22A 1 0.124013 0.435878 0.748091 -21.00000 0.09201 AFIX 137 H22D 2 0.127677 0.482461 0.735535 -21.00000 -1.50000 H22E 2 0.134593 0.440347 0.776503 -21.00000 -1.50000 H22F 2 0.072074 0.416840 0.744263 -21.00000 -1.50000 AFIX 0 C23A 1 0.136163 0.342924 0.699987 -21.00000 0.03219 AFIX 137 H23D 2 0.092927 0.320335 0.713685 -21.00000 -1.50000 H23E 2 0.169155 0.306545 0.688200 -21.00000 -1.50000 H23F 2 0.116448 0.373988 0.679084 -21.00000 -1.50000 AFIX 0 C21A 1 0.186340 0.349909 0.769557 -21.00000 0.05437 AFIX 137 H21D 2 0.140120 0.320992 0.773361 -21.00000 -1.50000 H21E 2 0.189235 0.385700 0.790495 -21.00000 -1.50000 H21F 2 0.232095 0.319673 0.770702 -21.00000 -1.50000 AFIX 0 HKLF 4 REM C:\XRay\TH153_~1\Pccn_a.res in Pccn REM wR2 = 0.2622, GooF = S = 1.002, Restrained GooF = 1.002 for all data REM R1 = 0.0792 for 5428 Fo > 4sig(Fo) and 0.1609 for all 10849 data REM 556 parameters refined using 17 restraints END WGHT 0.1470 0.0000 REM Highest difference peak 1.225, deepest hole -0.643, 1-sigma level 0.090 Q1 1 0.2428 0.7135 0.6445 11.00000 0.05 1.23 Q2 1 0.6588 0.3242 0.6561 11.00000 0.05 0.76 Q3 1 0.7264 0.3496 0.6231 11.00000 0.05 0.75 Q4 1 0.7500 0.2500 0.6489 10.50000 0.05 0.74 Q5 1 0.7112 0.1735 0.4981 11.00000 0.05 0.73 Q6 1 0.2789 0.6542 0.6236 11.00000 0.05 0.72 Q7 1 0.2837 0.7468 0.6088 11.00000 0.05 0.71 Q8 1 0.7458 0.2310 0.4975 11.00000 0.05 0.69 Q9 1 0.5334 1.0217 0.5527 11.00000 0.05 0.54 Q10 1 0.7539 0.1577 0.5325 11.00000 0.05 0.54 Q11 1 0.5021 0.9958 0.6312 11.00000 0.05 0.51 Q12 1 0.5441 1.0300 0.5866 11.00000 0.05 0.49 Q13 1 0.5774 1.0465 0.6108 11.00000 0.05 0.48 Q14 1 0.3636 0.1658 0.4922 11.00000 0.05 0.43 Q15 1 0.6908 0.2168 0.5202 11.00000 0.05 0.42 Q16 1 0.6473 0.6389 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7 20 75.39 7.10 9 12 30 -1.30 5.50 10 9 23 -2.00 5.40 11 8 18 8.60 5.20 11 10 23 1.70 6.00 11 11 25 -5.40 5.90 11 13 28 10.60 6.80 12 6 1 36.70 2.90 12 13 26 3.50 6.10 13 8 10 -0.80 4.80 13 9 14 5.40 5.50 13 11 20 -3.10 5.40 13 12 22 10.20 6.00 13 13 24 6.20 6.20 14 13 21 5.20 5.70 14 14 23 3.10 5.40 -11 5 24 12.80 4.90 -11 7 29 13.80 6.20 -9 3 20 46.20 5.20 -9 4 23 9.60 4.90 -9 5 26 4.70 4.70 -8 2 17 2.70 3.10 -8 4 24 7.80 4.90 -7 5 27 26.80 5.80 -6 9 35 4.40 5.60 -5 3 22 5.70 4.60 -4 3 22 33.20 4.30 -4 6 30 8.80 5.40 -4 7 32 2.40 6.00 -3 1 14 100.89 4.30 -3 7 32 2.80 5.70 -2 3 22 85.09 5.80 -2 4 25 6.20 4.50 -1 1 13 132.79 4.70 -1 5 27 -0.70 4.20 0 1 12 3.30 2.50 0 2 17 1.90 2.70 0 3 21 2.40 3.80 0 4 24 188.18 8.10 0 6 29 -5.10 5.30 1 2 16 100.29 4.60 1 3 20 4.40 3.20 1 5 26 15.60 4.70 1 11 37 -4.70 6.50 1 12 38 -4.90 4.70 2 2 15 5.10 2.90 2 3 19 26.40 3.90 3 3 18 144.49 6.30 3 6 27 15.10 5.50 3 7 29 4.10 4.80 4 2 11 174.08 5.10 4 4 20 244.18 7.90 4 7 28 4.80 4.80 4 8 30 10.80 5.10 5 8 29 8.90 4.60 5 11 34 7.30 5.20 6 2 3 44.30 2.30 6 3 12 4.10 3.20 8 3 2 30.30 2.40 8 5 16 73.19 5.60 9 4 7 20.30 3.20 9 5 13 42.10 4.40 9 6 17 45.60 5.00 9 8 23 2.10 5.40 10 5 9 84.09 4.80 10 6 14 113.19 6.40 10 8 21 4.30 5.40 11 6 10 -2.70 3.50 11 9 21 6.50 5.70 11 12 27 2.80 6.20 12 6 3 2.60 2.80 12 8 15 58.29 6.10 12 10 21 21.00 5.80 12 11 23 1.70 5.70 12 12 25 -4.70 6.10 13 9 15 0.70 5.60 14 9 10 12.00 5.10 14 11 17 -7.60 5.90 -11 6 27 3.40 5.50 -10 7 30 24.00 6.10 -8 3 21 7.30 3.60 -8 8 33 6.50 5.40 -7 1 13 52.49 3.10 -7 2 18 59.29 4.30 -6 3 22 -0.60 4.10 -6 6 30 -0.20 5.70 -6 7 32 7.10 5.90 -5 1 14 1.90 2.30 -5 5 28 -3.90 5.40 -5 8 34 5.20 6.10 -4 2 19 18.40 3.80 -4 5 28 0.80 4.80 -2 0 6 84.09 2.40 -2 1 14 119.39 4.70 -1 2 18 4.70 3.10 -1 3 22 117.19 6.70 -1 4 25 14.80 5.40 0 9 35 3.70 5.40 1 1 11 0.50 2.20 1 7 31 8.60 6.00 2 1 9 292.77 5.50 2 6 28 3.10 4.60 2 8 32 17.90 5.40 3 1 6 700.83 7.40 3 4 22 2.40 4.50 3 9 33 1.60 4.80 3 11 36 -2.10 5.00 4 3 17 25.60 4.00 5 2 9 17.00 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7 31 0.80 4.90 5 8 33 -1.50 4.90 6 11 37 3.90 5.30 7 4 19 15.40 5.00 7 8 31 7.60 5.80 8 3 9 21.00 3.10 9 5 18 40.90 5.90 9 6 22 14.70 5.20 10 4 4 54.69 3.40 10 4 5 -1.30 2.50 10 6 19 9.10 5.00 10 9 28 -7.10 6.20 10 11 32 10.40 6.90 11 5 9 3.80 3.40 11 6 16 3.30 5.00 11 7 20 11.80 5.50 11 8 23 9.90 5.50 11 9 26 10.10 5.60 11 10 28 3.40 6.60 11 11 30 0.20 6.70 12 7 16 27.20 5.00 12 8 20 26.40 5.70 12 11 28 6.20 6.10 13 7 11 2.60 5.00 13 9 20 -1.60 5.50 13 10 23 31.60 6.30 13 11 25 3.20 5.90 14 8 11 -1.30 4.80 14 9 16 1.50 5.60 15 12 21 3.50 6.00 -10 3 22 9.50 4.90 -9 2 19 6.40 3.60 -7 1 16 -1.80 2.80 -7 2 21 3.20 3.30 -7 3 25 6.10 4.60 -7 6 33 2.00 5.70 -6 1 17 126.49 5.20 -3 0 10 183.18 4.30 -2 9 39 1.00 5.40 0 0 6 9999.00 24.60 0 3 25 2.80 4.10 0 4 28 36.50 5.40 0 6 33 -1.10 4.90 0 7 35 -3.70 5.00 0 10 40 0.50 5.20 1 1 15 133.39 5.00 2 6 32 17.10 5.50 2 7 34 1.90 4.90 3 9 37 1.60 5.20 4 1 7 845.52 8.90 4 3 21 93.49 6.00 5 2 14 13.90 3.40 6 3 17 123.09 5.60 6 5 25 0.20 4.30 6 10 36 0.00 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-21 8 4.70 9.90 -2 -20 6 5.20 9.60 -2 -19 4 -2.30 9.60 -2 -18 3 28.50 10.10 -2 -17 2 52.59 10.10 -2 -16 1 3.70 9.60 -2 -15 0 5.50 7.20 -2 -12 -1 11.60 6.90 -2 -10 -1 292.77 11.10 -2 -9 -1 1.40 4.40 -2 -5 1 32.20 3.90 -2 -3 3 54.99 3.50 -1 -23 7 -8.00 9.70 -1 -21 3 -3.50 9.10 -1 -20 2 3.10 9.90 -1 -15 -3 -7.20 6.90 -1 -12 -4 -5.50 6.60 -1 -11 -4 12.70 6.00 -1 -10 -4 7.70 5.60 -1 -9 -4 142.69 7.60 0 -24 5 -4.80 9.80 0 -23 3 5.50 9.20 0 -21 0 1.70 9.70 0 -16 -5 8.40 8.50 0 -14 -6 203.98 11.70 0 -7 -6 -4.00 3.80 0 -5 -5 5.90 2.50 1 -24 2 -10.30 12.10 1 -23 0 -13.60 12.10 1 -21 -3 -4.70 9.80 1 -20 -4 0.20 9.30 1 -19 -5 181.48 13.50 1 -18 -6 7.70 9.50 2 -24 -1 -2.30 12.00 2 -22 -4 -10.10 10.80 2 -18 -8 7.10 8.70 2 -17 -9 11.00 6.90 2 -15 -10 1.50 7.10 3 -18 -10 4.40 8.80 3 -14 -12 86.39 9.10 3 -7 -12 35.50 4.40 4 -23 -7 10.60 11.10 4 -22 -8 -4.30 10.90 4 -19 -11 11.50 9.50 4 -16 -13 11.10 7.40 4 -13 -14 8.10 6.50 4 -12 -14 17.50 6.70 5 -22 -10 -2.90 10.10 5 -21 -11 -13.60 9.10 5 -17 -14 10.00 7.60 6 -23 -10 -9.90 10.20 6 -19 -14 5.10 8.30 6 -15 -16 3.80 6.70 6 -6 -16 5.70 3.40 7 -12 -18 -4.00 5.50 7 -11 -18 42.60 6.40 7 -10 -18 20.80 4.70 8 -18 -17 2.30 8.10 8 -16 -18 11.50 7.40 -5 -15 21 7.20 9.10 -5 -15 22 24.30 9.50 -5 -15 23 14.10 10.10 -5 -15 24 0.30 9.10 -5 -14 18 44.90 9.20 -5 -14 19 3.00 8.20 -5 -14 27 3.10 10.00 -5 -13 16 22.30 8.50 -5 -12 16 23.00 8.40 -5 -11 15 17.90 8.00 -5 -10 15 10.30 6.70 -5 -7 18 74.49 7.60 -5 -6 22 8.90 4.80 -5 -6 23 9.70 5.50 -4 -19 20 6.00 9.80 -4 -19 21 -2.50 10.50 -4 -19 22 -5.10 10.80 -4 -19 23 1.80 9.60 -4 -19 24 -5.70 10.40 -4 -19 25 -6.30 10.20 -4 -19 26 0.80 9.40 -4 -18 15 -10.80 8.50 -4 -18 16 6.10 10.00 -4 -17 13 35.80 10.30 -4 -13 8 84.09 9.00 -4 -12 8 58.59 9.00 -4 -5 11 179.58 7.30 -3 -21 16 -2.20 11.70 -3 -19 10 20.30 10.50 -3 -18 8 38.80 10.50 -3 -14 4 -2.40 8.30 -3 -11 3 18.90 6.40 -3 -10 3 83.69 7.80 -3 -9 3 22.90 5.70 -2 -23 15 6.20 12.00 -2 -22 11 23.80 12.20 -2 -19 5 -4.20 9.60 -2 -14 0 36.70 7.60 -2 -7 0 2.00 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28 5.40 8.70 -1 -12 29 9.60 9.80 -1 -10 11 358.96 12.20 -1 -9 9 -3.40 4.50 0 -14 17 4.00 8.00 0 -14 30 -3.80 9.50 0 -13 13 1.10 7.90 0 -12 10 785.32 19.60 0 -10 6 20.50 6.10 1 -16 18 -1.70 8.00 1 -16 19 6.50 10.40 1 -16 27 -1.20 9.10 1 -16 28 -0.30 10.40 1 -16 29 0.00 9.50 1 -13 7 324.07 14.10 1 -12 5 21.60 7.40 1 -10 2 -1.10 5.40 2 -17 15 9.10 9.20 2 -16 11 49.40 10.30 2 -14 5 86.39 9.20 2 -13 3 46.20 7.70 2 -11 0 -2.50 5.70 3 -19 21 6.20 10.10 3 -19 22 -1.50 11.00 3 -19 23 4.40 11.10 3 -19 24 -5.80 11.30 3 -19 25 -2.30 11.30 3 -19 26 3.00 10.80 3 -19 27 9.70 9.80 3 -18 13 -2.30 8.60 3 -17 9 4.30 9.20 3 -16 6 9.50 8.30 3 -13 0 230.88 12.10 4 -20 22 -4.60 11.90 4 -20 23 0.10 11.70 4 -19 12 2.10 8.60 4 -18 8 11.10 8.40 4 -17 5 9.90 8.00 4 -14 -1 15.30 7.80 4 -12 -4 117.69 9.40 5 -21 19 9.40 12.50 5 -20 12 -4.70 10.80 5 -19 8 -1.30 10.00 5 -17 2 21.00 9.30 5 -16 0 3.90 9.10 5 -15 -2 56.19 8.80 5 -12 -6 51.89 7.60 5 -9 -9 2.70 4.50 6 -20 8 -3.90 10.10 6 -15 -4 4.30 8.60 6 -12 -8 23.10 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7.70 6.50 3 -11 31 5.40 9.00 3 -10 8 17.40 6.40 3 -7 0 1055.69 16.00 4 -12 12 8.40 7.70 4 -12 32 3.90 8.90 5 -13 11 6.80 7.40 5 -13 12 64.79 10.20 5 -13 32 3.10 9.30 5 -12 7 99.59 10.60 5 -12 37 -0.10 11.20 6 -14 32 10.50 9.70 6 -7 -7 75.19 5.70 7 -15 13 35.70 9.50 7 -15 30 -4.20 11.00 7 -15 31 0.10 10.50 7 -14 8 129.09 12.10 7 -13 4 74.69 10.30 7 -12 1 21.40 7.80 7 -10 -4 8.40 5.50 8 -16 16 0.30 10.00 8 -16 17 -8.30 9.40 8 -16 27 -12.40 11.20 8 -16 28 18.30 11.80 8 -15 9 12.50 10.10 8 -8 -9 62.59 6.00 9 -16 11 1.20 10.40 9 -15 6 -5.20 9.00 9 -14 2 18.80 8.80 9 -13 -1 8.20 7.50 9 -9 -9 11.20 5.30 9 -5 -14 -1.40 4.00 10 -17 14 4.10 10.30 10 -14 0 66.39 10.20 10 -12 -5 93.19 10.00 10 -11 -7 29.20 7.40 10 -7 -13 49.10 6.20 10 -4 -16 2.00 3.50 11 -18 20 -4.90 10.10 11 -17 10 16.40 9.80 11 -16 5 10.70 9.60 11 -13 -4 7.50 8.50 11 -10 -10 2.00 7.00 11 -7 -14 45.30 6.10 12 -18 14 4.40 11.20 12 -18 15 -4.50 11.00 12 -17 7 -8.00 8.80 12 -16 3 17.10 10.80 12 -15 0 -2.00 10.00 12 -14 -3 10.80 9.50 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6.40 -11 -14 3 6.20 5.70 -11 -8 -3 35.30 6.40 -11 -4 -11 72.19 6.90 -11 -2 -18 1.10 5.00 -11 -1 -30 2.90 5.80 -11 -1 -28 -3.20 6.10 -11 -1 -27 -3.60 5.30 -11 -1 -26 0.90 5.60 -10 -17 6 -4.80 6.20 -10 -1 -18 14.60 5.40 -10 0 -28 79.89 7.30 -10 0 -27 0.50 5.80 -10 0 -26 -3.60 5.40 -9 -19 8 -3.00 6.10 -9 -18 8 5.60 5.50 -9 -15 7 54.99 6.70 -9 -13 6 3.80 4.90 -9 -7 0 186.58 7.70 -9 -2 -10 17.30 4.10 -9 0 -18 69.19 5.50 -9 1 -28 2.80 5.40 -8 -14 8 36.00 5.50 -8 -11 6 51.19 5.70 -8 -8 3 15.90 4.00 -8 -4 -3 130.19 6.20 -8 -3 -5 161.38 6.60 -8 0 -14 10.00 3.60 -7 -4 -1 14.30 3.30 -6 -15 11 113.59 6.70 -6 -10 8 -0.10 3.20 -6 -8 6 16.50 3.60 -6 2 -16 4.90 3.10 -6 3 -24 3.40 3.10 -5 -11 10 23.60 4.00 -5 -6 5 230.08 6.30 -5 -4 2 41.50 3.00 -4 -11 11 49.60 4.20 -4 4 -22 22.80 2.70 -3 4 -18 46.30 2.70 -16 -15 -11 15.10 7.30 -16 -14 -12 -2.10 6.40 -16 -11 -16 4.00 8.10 -16 -10 -19 8.70 8.50 -16 -9 -23 1.80 7.90 -16 -9 -22 5.50 8.10 -15 -18 -5 1.20 8.00 -15 -16 -6 7.00 8.40 -15 -11 -11 8.80 7.20 -15 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4.70 6.20 -14 11 23 -3.00 6.20 -14 14 14 -5.60 4.80 -14 15 10 -4.70 5.90 -14 16 2 15.30 5.60 -14 16 3 8.60 5.40 -13 7 29 -5.30 5.80 -13 12 19 2.80 5.70 -13 13 16 18.20 5.90 -13 14 12 -2.00 5.10 -13 15 7 0.80 5.60 -12 0 35 1.10 3.50 -12 8 26 -1.70 5.40 -12 10 22 -3.80 4.30 -12 11 20 5.40 5.50 -12 12 17 -0.50 4.50 -12 13 14 13.80 5.50 -12 15 2 29.20 5.50 -12 15 3 7.80 5.20 -11 0 34 -0.10 3.80 -11 5 29 -4.10 4.30 -11 6 28 8.50 4.70 -11 11 18 10.40 5.40 -11 12 15 2.40 5.10 -11 14 6 2.60 5.40 -10 1 32 -2.50 3.90 -10 3 30 5.30 4.30 -10 4 29 7.40 5.00 -10 8 23 23.40 5.50 -10 11 16 5.60 5.20 -10 14 -9 20.10 4.50 -10 14 -8 8.80 4.40 -10 14 -1 9.00 4.50 -9 -1 32 2.30 4.10 -9 5 26 -0.50 4.70 -9 7 23 11.70 5.20 -9 8 21 6.30 4.60 -9 10 16 21.50 4.80 -9 12 9 -0.90 4.40 -9 13 -12 -1.30 4.00 -9 13 2 10.70 4.20 -9 13 3 -0.40 4.50 -8 -2 31 1.10 4.00 -8 1 29 11.00 4.10 -8 2 28 54.29 5.50 -8 3 27 32.50 5.00 -8 7 21 4.50 4.40 -8 12 4 12.40 4.20 -7 -3 30 23.00 4.30 -7 0 28 -4.00 3.70 -7 1 27 24.40 4.30 -7 2 26 142.99 6.60 -7 3 25 2.40 4.40 -7 8 16 -1.40 3.60 -7 9 13 8.80 3.60 -7 10 10 2.00 3.90 -7 11 -14 26.20 3.00 -6 0 26 12.10 3.60 -6 1 25 76.59 5.30 -6 9 9 4.80 3.20 -6 10 4 -4.20 2.80 -5 -5 27 -0.20 1.70 -5 -3 26 12.10 3.40 -5 9 3 -5.40 2.90 -4 -2 23 8.80 3.00 -4 -1 22 14.00 2.70 -4 1 20 22.00 3.10 -4 3 17 27.80 3.20 -4 5 13 342.27 7.20 -4 8 -10 295.57 4.80 -3 -2 20 4.90 2.10 -3 0 18 33.40 2.90 -3 4 11 423.66 7.10 -3 5 8 10.20 2.30 -3 6 4 21.60 2.50 -2 4 5 741.03 7.80 -2 5 -2 188.58 3.50 -1 1 7 134.79 2.90 -16 14 18 4.30 6.50 -16 16 10 26.10 6.70 -16 17 2 1.40 5.70 -16 17 3 2.30 5.60 -15 12 22 1.10 5.50 -15 13 20 6.50 6.10 -15 16 7 4.70 5.20 -14 5 33 2.80 5.10 -14 12 21 6.80 5.70 -14 13 18 -4.70 5.10 -14 14 15 6.70 6.50 -14 16 4 21.40 5.40 -14 16 5 10.00 5.80 -13 2 35 2.20 4.10 -13 3 34 1.40 4.70 -13 4 33 15.60 4.90 -13 5 32 7.50 5.60 -13 9 26 7.30 5.00 -13 10 24 4.20 4.60 -13 11 22 -6.80 5.30 -13 14 13 3.80 5.30 -13 15 8 13.70 5.80 -13 16 -6 -7.50 5.20 -13 16 -5 -2.10 5.30 -13 16 -4 -5.90 4.90 -13 16 -3 2.70 5.00 -13 16 -2 0.90 4.90 -13 16 -1 13.10 5.30 -12 2 34 5.60 4.20 -12 3 33 -1.80 4.70 -12 4 32 8.50 4.90 -12 5 31 4.10 4.70 -12 7 28 -7.00 4.60 -12 9 25 1.00 5.20 -12 10 23 0.20 5.00 -12 12 18 46.40 6.30 -12 15 4 1.50 5.10 -11 8 25 29.80 5.10 -11 9 23 6.30 4.50 -11 10 21 23.20 5.00 -11 12 16 5.20 5.00 -11 13 12 -0.70 5.10 -11 14 7 17.50 5.40 -10 0 33 0.10 4.00 -10 5 28 6.40 4.60 -10 10 19 92.29 6.60 -10 12 13 21.10 5.00 -10 14 -10 71.59 6.00 -10 14 1 5.40 4.60 -10 14 2 5.50 4.70 -9 -2 33 5.80 3.80 -9 2 30 18.10 4.40 -9 3 29 6.50 4.40 -9 10 17 40.50 5.80 -9 12 10 3.30 5.10 -9 13 4 4.70 4.70 -8 0 30 6.80 3.90 -8 4 26 1.00 4.70 -8 9 17 6.50 4.50 -8 10 14 21.20 5.00 -8 11 10 27.40 4.60 -7 -1 29 13.40 3.90 -7 4 24 -1.20 4.20 -7 7 19 87.39 6.00 -6 -1 27 3.10 3.30 -6 3 23 23.90 4.10 -6 5 20 1.90 3.70 -6 6 18 13.10 3.60 -6 7 16 13.30 4.40 -6 8 13 179.68 6.60 -6 9 10 4.80 4.10 -6 10 5 570.54 9.90 -5 0 24 2.90 2.80 -5 1 23 2.80 3.10 -5 4 19 10.60 3.30 -5 5 17 79.69 4.40 -5 8 9 -0.70 2.80 -5 9 4 643.14 10.00 -4 2 19 20.40 3.30 -4 6 11 1.20 3.00 -4 7 7 3.40 2.20 -4 8 2 147.59 5.00 -3 1 17 28.80 2.80 -2 1 13 182.18 4.50 -2 2 11 7.80 2.00 -2 5 -1 31.00 1.90 -1 2 4 131.79 2.70 -16 15 15 -6.10 6.50 -16 16 11 3.50 6.20 -16 17 4 9.20 6.30 -15 10 27 4.00 6.70 -15 11 25 -3.80 6.40 -15 12 23 6.50 6.10 -15 14 17 10.50 5.50 -15 15 14 7.80 6.80 -15 16 9 -1.90 6.20 -15 17 -4 1.80 5.40 -15 17 -3 -1.20 4.70 -15 17 -2 3.30 4.90 -15 17 -1 -1.30 4.60 -15 17 0 20.60 5.90 -14 6 32 2.80 4.60 -14 7 31 0.40 5.30 -14 9 28 0.90 6.30 -14 10 26 -0.30 6.20 -14 11 24 2.10 5.90 -14 14 16 2.70 6.20 -14 16 6 -3.30 5.60 -13 6 31 5.00 4.60 -13 7 30 1.00 5.40 -13 13 17 -3.20 4.70 -13 15 9 17.10 5.90 -13 16 0 0.60 4.80 -13 16 1 7.50 5.30 -12 1 35 2.30 4.00 -12 6 30 4.80 5.40 -12 11 21 5.20 5.30 -12 13 15 3.60 4.70 -12 15 6 4.70 5.20 -11 1 34 -1.10 4.20 -11 2 33 8.70 4.40 -11 3 32 22.10 4.80 -11 4 31 6.10 4.70 -11 5 30 0.40 4.90 -11 11 19 -1.20 4.50 -11 13 13 75.69 6.60 -11 14 8 9.20 5.20 -11 15 -7 -2.00 4.70 -11 15 -6 -8.20 4.90 -11 15 -5 11.40 4.50 -11 15 -4 43.40 5.50 -11 15 -3 6.20 4.70 -11 15 -2 1.90 4.90 -11 15 -1 60.49 6.00 -10 -1 34 -0.20 3.60 -10 6 27 -3.40 4.10 -10 8 24 15.60 5.00 -10 9 22 20.40 5.60 -10 11 17 19.50 5.30 -10 12 14 36.80 5.90 -10 13 10 1.00 4.80 -10 14 3 46.30 6.00 -9 0 32 22.20 4.50 -9 1 31 3.60 4.00 -9 4 28 -1.70 4.50 -9 5 27 -0.30 4.50 -9 7 24 48.60 5.80 -9 8 22 8.30 5.10 -9 9 20 20.10 5.30 -9 12 11 10.00 5.00 -9 13 5 8.80 4.50 -8 -1 31 51.29 5.60 -8 5 25 15.40 4.90 -8 11 11 73.49 5.90 -7 -2 30 36.50 4.70 -7 6 21 15.20 4.00 -7 8 17 0.70 3.70 -7 10 11 8.60 4.30 -7 11 6 83.29 5.20 -6 -4 29 10.90 3.60 -6 -2 28 25.90 4.30 -6 8 14 16.90 4.40 -6 10 6 38.10 4.20 -5 -1 25 2.90 2.60 -5 2 22 86.59 4.70 -5 7 13 108.59 5.30 -5 9 5 0.10 3.00 -4 -3 24 -0.60 2.70 -4 4 16 -1.40 2.90 -4 5 14 3.90 3.00 -4 7 8 13.40 3.10 -3 3 14 670.13 9.30 -3 5 9 3.70 2.00 -3 6 5 6.80 2.00 -2 -2 17 375.06 5.70 -2 -1 16 54.89 2.70 -2 3 9 260.67 5.10 -2 5 0 -1.60 1.40 -16 17 6 6.90 5.90 -15 13 21 9.90 6.50 -15 14 18 1.90 6.20 -15 16 10 0.90 6.20 -15 17 1 -1.90 5.00 -15 17 2 -2.30 5.00 -14 12 22 -6.30 5.40 -13 9 27 -9.60 6.30 -13 10 25 10.90 5.10 -13 11 23 14.30 5.00 -13 12 21 11.10 5.80 -13 13 18 -1.40 5.50 -13 15 10 6.30 5.80 -13 16 2 2.70 4.80 -13 16 3 -3.80 5.30 -12 0 36 4.60 4.60 -12 7 29 6.00 5.10 -12 10 24 10.30 5.20 -12 12 19 7.90 5.60 -12 13 16 10.00 5.30 -12 14 12 9.20 5.20 -12 15 7 7.70 5.70 -11 6 29 5.90 4.80 -11 8 26 -3.00 4.80 -11 9 24 0.40 4.30 -11 10 22 -0.20 4.30 -11 11 20 0.00 5.20 -11 12 17 16.30 5.40 -11 15 -8 25.70 5.00 -11 15 0 38.70 5.80 -11 15 1 69.59 6.20 -11 15 2 4.20 5.00 -10 2 32 2.80 4.30 -10 3 31 13.10 4.70 -10 5 29 -1.70 4.60 -10 14 4 1.00 4.30 -10 14 5 26.50 5.20 -9 6 26 -3.30 4.60 -9 10 18 -0.30 5.20 -9 11 15 -2.80 4.90 -8 2 29 20.70 4.50 -8 3 28 9.20 4.20 -8 7 22 0.70 3.70 -8 8 20 114.39 6.40 -8 9 18 7.30 5.10 -8 10 15 38.30 5.10 -8 11 12 56.69 5.80 -7 1 28 12.90 4.20 -7 2 27 -6.00 4.20 -7 3 26 -1.20 4.30 -7 9 15 12.70 4.90 -7 10 12 25.60 4.70 -7 11 7 2.20 3.30 -7 12 -5 32.40 3.70 -7 12 -4 1.60 3.10 -7 12 -3 5.70 3.30 -6 2 25 8.50 3.90 -6 6 19 279.57 8.40 -6 9 11 11.10 3.50 -6 10 7 61.39 5.00 -6 11 -4 17.00 3.20 -6 11 -3 36.00 3.70 -5 -2 26 68.29 4.50 -5 3 21 3.40 3.10 -5 5 18 191.98 6.80 -5 8 10 -3.20 2.70 -5 9 6 50.69 4.10 -4 8 3 293.57 6.30 -3 4 12 213.28 5.30 -3 6 6 11.70 2.70 -3 7 -4 465.55 6.20 -2 0 15 -0.50 1.80 -2 4 6 1669.43 12.00 -2 5 1 32.30 2.10 -15 11 26 -1.20 5.40 -15 15 15 5.70 5.30 -14 13 20 0.30 5.20 -14 14 17 2.10 5.10 -12 11 22 23.50 5.50 -10 11 18 23.00 5.20 -10 12 15 49.70 5.60 -10 13 11 6.10 4.30 -9 12 12 112.89 6.50 -7 7 20 19.40 4.30 -4 6 12 8.10 2.70 -4 8 4 32.60 2.80 -1 2 5 70.69 2.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 78132 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' '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 0.46073(4) 0.53029(4) 0.60429(2) 0.0525(2) Uani 1 1 d . . . . . Cl2 Cl 0.37313(8) 0.13325(8) 0.50135(4) 0.0479(4) Uani 1 1 d . . . . . P03 P 0.56803(8) 0.58206(9) 0.64199(4) 0.0449(4) Uani 1 1 d . . . . . P004 P 0.44719(8) 0.41985(9) 0.64232(5) 0.0486(4) Uani 1 1 d . . . . . Cl1 Cl 0.54104(11) 0.47773(11) 0.55867(5) 0.0774(6) Uani 1 1 d . . . . . O1 O 0.45326(19) 0.5388(2) 0.69027(11) 0.0459(10) Uani 1 1 d . . . . . N3 N 0.3262(3) 0.3876(3) 0.58478(15) 0.0509(13) Uani 1 1 d . . . . . N4 N 0.4151(3) 0.3078(3) 0.59078(15) 0.0529(13) Uani 1 1 d . . . . . N1 N 0.5759(3) 0.6858(3) 0.57776(14) 0.0495(12) Uani 1 1 d . . . . . N2 N 0.6822(3) 0.6281(3) 0.58947(15) 0.0526(13) Uani 1 1 d . . . . . C1 C 0.4579(3) 0.6110(3) 0.69641(17) 0.0436(13) Uani 1 1 d . . . . . C2 C 0.5137(3) 0.6448(3) 0.67310(17) 0.0459(15) Uani 1 1 d . . . . . C3 C 0.5259(3) 0.7164(3) 0.67991(17) 0.0490(15) Uani 1 1 d . . . . . H3 H 0.563845 0.740779 0.664962 0.059 Uiso 1 1 calc R U . . . C24 C 0.6069(3) 0.6376(3) 0.60234(17) 0.0474(15) Uani 1 1 d . . . . . C4 C 0.4821(3) 0.7541(4) 0.70916(19) 0.0519(16) Uani 1 1 d . . . . . C33 C 0.3925(3) 0.3707(4) 0.60468(18) 0.0517(15) Uani 1 1 d . . . . . C13 C 0.3844(3) 0.5059(3) 0.69893(17) 0.0461(14) Uani 1 1 d . . . . . C6 C 0.4117(3) 0.6451(4) 0.72396(17) 0.0478(15) Uani 1 1 d . . . . . C12 C 0.3707(3) 0.4454(3) 0.67714(17) 0.0481(15) Uani 1 1 d . . . . . C8 C 0.3339(3) 0.5347(4) 0.72683(17) 0.0510(16) Uani 1 1 d . . . . . C11 C 0.3035(3) 0.4063(4) 0.68708(18) 0.0555(17) Uani 1 1 d . . . . . H11 H 0.293537 0.362983 0.673790 0.067 Uiso 1 1 calc R U . . . C7 C 0.3538(3) 0.6028(4) 0.74854(17) 0.0528(16) Uani 1 1 d . . . . . C5 C 0.4272(3) 0.7164(4) 0.72981(19) 0.0551(16) Uani 1 1 d . . . . . H5 H 0.398074 0.740767 0.749315 0.066 Uiso 1 1 calc R U . . . C9 C 0.2680(3) 0.4939(4) 0.7340(2) 0.0609(18) Uani 1 1 d . . . . . H9 H 0.231607 0.511239 0.752648 0.073 Uiso 1 1 calc R U . . . C36 C 0.2816(3) 0.4541(3) 0.58672(19) 0.0552(16) Uani 1 1 d . . . . . H36 H 0.305330 0.485087 0.607387 0.066 Uiso 1 1 calc R U . . . C10 C 0.2523(3) 0.4297(4) 0.71563(19) 0.0582(17) Uani 1 1 d . . . . . C27 C 0.7399(3) 0.5799(4) 0.60631(19) 0.0582(17) Uani 1 1 d . . . . . H27 H 0.717759 0.557856 0.630728 0.070 Uiso 1 1 calc R U . . . C39 C 0.4864(4) 0.2681(4) 0.60256(19) 0.0584(17) Uani 1 1 d . . . . . H39 H 0.510118 0.292793 0.625742 0.070 Uiso 1 1 calc R U . . . C34 C 0.3096(4) 0.3342(4) 0.55850(19) 0.0600(17) Uani 1 1 d . . . . . H34 H 0.266930 0.332715 0.540927 0.072 Uiso 1 1 calc R U . . . C37 C 0.2863(4) 0.4921(4) 0.5471(2) 0.070(2) Uani 1 1 d . . . . . H37A H 0.340373 0.498634 0.539715 0.105 Uiso 1 1 calc R U . . . H37B H 0.261192 0.538391 0.549251 0.105 Uiso 1 1 calc R U . . . H37C H 0.260211 0.463935 0.526758 0.105 Uiso 1 1 calc R U . . . C16 C 0.4996(3) 0.8328(3) 0.71730(17) 0.0599(17) Uani 1 1 d D . . . . C21 C 0.2033(9) 0.3540(10) 0.7693(3) 0.069(5) Uani 0.843(14) 1 d D . P A 1 H21A H 0.158473 0.329240 0.780172 0.104 Uiso 0.843(14) 1 calc R U P A 1 H21B H 0.219152 0.391498 0.787590 0.104 Uiso 0.843(14) 1 calc R U P A 1 H21C H 0.245793 0.320382 0.765887 0.104 Uiso 0.843(14) 1 calc R U P A 1 C35 C 0.3648(4) 0.2843(4) 0.5620(2) 0.0666(19) Uani 1 1 d . . . . . H35 H 0.368207 0.241396 0.547553 0.080 Uiso 1 1 calc R U . . . C32 C 0.4884(4) 0.7881(4) 0.5792(2) 0.078(2) Uani 1 1 d . . . . . H32A H 0.515976 0.804483 0.602780 0.117 Uiso 1 1 calc R U . . . H32B H 0.434259 0.802402 0.580911 0.117 Uiso 1 1 calc R U . . . H32C H 0.511690 0.808996 0.555482 0.117 Uiso 1 1 calc R U . . . C30 C 0.4933(4) 0.7084(4) 0.5767(2) 0.0617(18) Uani 1 1 d . . . . . H30 H 0.465942 0.687486 0.599955 0.074 Uiso 1 1 calc R U . . . C38 C 0.1985(4) 0.4391(4) 0.5987(2) 0.0688(19) Uani 1 1 d . . . . . H38A H 0.172382 0.413728 0.577220 0.103 Uiso 1 1 calc R U . . . H38B H 0.171779 0.483869 0.603719 0.103 Uiso 1 1 calc R U . . . H38C H 0.197849 0.410182 0.622746 0.103 Uiso 1 1 calc R U . . . C14 C 0.2809(3) 0.6465(4) 0.7566(2) 0.069(2) Uani 1 1 d . . . . . H14A H 0.257081 0.659927 0.731340 0.103 Uiso 1 1 calc R U . . . H14B H 0.294559 0.689192 0.771430 0.103 Uiso 1 1 calc R U . . . H14C H 0.244409 0.618247 0.772082 0.103 Uiso 1 1 calc R U . . . C25 C 0.6945(4) 0.6701(4) 0.5570(2) 0.0606(17) Uani 1 1 d . . . . . H25 H 0.740910 0.673233 0.542204 0.073 Uiso 1 1 calc R U . . . C26 C 0.6284(4) 0.7067(4) 0.5498(2) 0.0641(18) Uani 1 1 d . . . . . H26 H 0.620211 0.740227 0.529252 0.077 Uiso 1 1 calc R U . . . C15 C 0.3906(4) 0.5828(4) 0.78875(18) 0.0636(18) Uani 1 1 d . . . . . H15A H 0.352544 0.558024 0.805115 0.095 Uiso 1 1 calc R U . . . H15B H 0.407504 0.625738 0.802411 0.095 Uiso 1 1 calc R U . . . H15C H 0.434939 0.551826 0.784184 0.095 Uiso 1 1 calc R U . . . C29 C 0.7588(4) 0.5225(4) 0.5777(2) 0.074(2) Uani 1 1 d . . . . . H29A H 0.711495 0.497677 0.570056 0.110 Uiso 1 1 calc R U . . . H29B H 0.794509 0.489012 0.590042 0.110 Uiso 1 1 calc R U . . . H29C H 0.782802 0.542966 0.554024 0.110 Uiso 1 1 calc R U . . . C20 C 0.1826(4) 0.3861(4) 0.72941(19) 0.075(2) Uani 1 1 d D . . . . O2 O 0.250000 0.750000 0.6098(4) 0.173(5) Uiso 1 2 d S . P . . C28 C 0.8106(4) 0.6242(4) 0.6183(2) 0.078(2) Uani 1 1 d . . . . . H28A H 0.832748 0.646485 0.594707 0.117 Uiso 1 1 calc R U . . . H28B H 0.849181 0.593376 0.630630 0.117 Uiso 1 1 calc R U . . . H28C H 0.794962 0.660748 0.637207 0.117 Uiso 1 1 calc R U . . . C31 C 0.4558(5) 0.6806(5) 0.5384(3) 0.099(3) Uani 1 1 d . . . . . H31A H 0.477200 0.705919 0.515565 0.148 Uiso 1 1 calc R U . . . H31B H 0.400086 0.688357 0.539572 0.148 Uiso 1 1 calc R U . . . H31C H 0.466331 0.629982 0.535687 0.148 Uiso 1 1 calc R U . . . C19 C 0.4595(6) 0.8616(6) 0.7541(3) 0.094(4) Uani 0.843(14) 1 d D . P A 1 H19A H 0.477613 0.909689 0.759423 0.140 Uiso 0.843(14) 1 calc R U P A 1 H19B H 0.471331 0.831232 0.776843 0.140 Uiso 0.843(14) 1 calc R U P A 1 H19C H 0.403705 0.862236 0.749734 0.140 Uiso 0.843(14) 1 calc R U P A 1 C40 C 0.4664(5) 0.1953(5) 0.6147(3) 0.118(4) Uani 1 1 d . . . . . H40A H 0.432448 0.197004 0.637896 0.177 Uiso 1 1 calc R U . . . H40B H 0.513556 0.169527 0.621506 0.177 Uiso 1 1 calc R U . . . H40C H 0.440103 0.171262 0.592900 0.177 Uiso 1 1 calc R U . . . C48 C 0.5168(6) 1.0055(6) 0.5900(4) 0.113(3) Uiso 1 1 d . . . . . C41 C 0.5431(5) 0.2689(6) 0.5692(3) 0.124(4) Uani 1 1 d . . . . . H41A H 0.589870 0.243643 0.577164 0.186 Uiso 1 1 calc R U . . . H41B H 0.556072 0.317842 0.562479 0.186 Uiso 1 1 calc R U . . . H41C H 0.520502 0.245581 0.545977 0.186 Uiso 1 1 calc R U . . . C47 C 0.4905(6) 0.9896(6) 0.5531(3) 0.117(3) Uiso 1 1 d . . . . . H47A H 0.447520 0.956222 0.555119 0.176 Uiso 1 1 calc R U . . . H47B H 0.532053 0.968237 0.537506 0.176 Uiso 1 1 calc R U . . . H47C H 0.472862 1.032909 0.539949 0.176 Uiso 1 1 calc R U . . . C18 C 0.5853(3) 0.8434(5) 0.7253(3) 0.079(3) Uani 0.843(14) 1 d D . P A 1 H18A H 0.596813 0.894083 0.726415 0.118 Uiso 0.843(14) 1 calc R U P A 1 H18B H 0.615348 0.821441 0.704075 0.118 Uiso 0.843(14) 1 calc R U P A 1 H18C H 0.598805 0.821481 0.750722 0.118 Uiso 0.843(14) 1 calc R U P A 1 C46 C 0.7163(5) 0.2314(6) 0.5158(3) 0.115(3) Uiso 1 1 d D . . . . H46A H 0.684463 0.248253 0.493373 0.138 Uiso 1 1 calc R U . . . H46B H 0.688098 0.242696 0.540510 0.138 Uiso 1 1 calc R U . . . C17 C 0.4769(10) 0.8787(5) 0.6821(3) 0.122(6) Uani 0.843(14) 1 d D . P A 1 H17A H 0.423341 0.868871 0.674789 0.184 Uiso 0.843(14) 1 calc R U P A 1 H17B H 0.510593 0.868037 0.659568 0.184 Uiso 0.843(14) 1 calc R U P A 1 H17C H 0.482165 0.928666 0.689219 0.184 Uiso 0.843(14) 1 calc R U P A 1 C43 C 0.2360(7) 0.6322(7) 0.6336(4) 0.151(4) Uiso 1 1 d D . . . . H43A H 0.209918 0.643830 0.658492 0.226 Uiso 1 1 calc R U . . . H43B H 0.262974 0.586952 0.636445 0.226 Uiso 1 1 calc R U . . . H43C H 0.197918 0.628514 0.612269 0.226 Uiso 1 1 calc R U . . . N5 N 0.5357(7) 1.0198(7) 0.6198(5) 0.184(5) Uiso 1 1 d . . . . . C23 C 0.1722(9) 0.3221(7) 0.7026(4) 0.157(8) Uani 0.843(14) 1 d D . P A 1 H23A H 0.130273 0.292563 0.712756 0.236 Uiso 0.843(14) 1 calc R U P A 1 H23B H 0.219978 0.294619 0.702006 0.236 Uiso 0.843(14) 1 calc R U P A 1 H23C H 0.159586 0.337960 0.675700 0.236 Uiso 0.843(14) 1 calc R U P A 1 C22 C 0.1096(5) 0.4308(7) 0.7301(7) 0.197(12) Uani 0.843(14) 1 d D . P A 1 H22A H 0.097691 0.446914 0.703225 0.296 Uiso 0.843(14) 1 calc R U P A 1 H22B H 0.117387 0.471794 0.747397 0.296 Uiso 0.843(14) 1 calc R U P A 1 H22C H 0.066721 0.402315 0.740229 0.296 Uiso 0.843(14) 1 calc R U P A 1 C42 C 0.2933(12) 0.6894(10) 0.6237(7) 0.294(11) Uiso 1 1 d D . . . . H42A H 0.323583 0.702136 0.647485 0.353 Uiso 1 1 calc R U . . . H42B H 0.329164 0.672879 0.602873 0.353 Uiso 1 1 calc R U . . . C45 C 0.7235(11) 0.1523(6) 0.5127(6) 0.246(9) Uiso 1 1 d D . . . . H45A H 0.755381 0.133960 0.534786 0.295 Uiso 1 1 calc R U . . . H45B H 0.748699 0.139309 0.487428 0.295 Uiso 1 1 calc R U . . . C44 C 0.6430(11) 0.1203(13) 0.5146(6) 0.300(11) Uiso 1 1 d D . . . . H44A H 0.604573 0.157943 0.512265 0.450 Uiso 1 1 calc R U . . . H44B H 0.636316 0.095749 0.539939 0.450 Uiso 1 1 calc R U . . . H44C H 0.636489 0.086597 0.492801 0.450 Uiso 1 1 calc R U . . . C49 C 0.6815(11) 0.3053(12) 0.6464(6) 0.252(9) Uiso 1 1 d D . . . . N6 N 0.6460(10) 0.2656(7) 0.6622(5) 0.232(6) Uiso 1 1 d D . . . . C50 C 0.6830(10) 0.3868(8) 0.6405(5) 0.244(9) Uiso 1 1 d D . . . . H50A H 0.652967 0.399168 0.616900 0.366 Uiso 1 1 calc R U . . . H50B H 0.736322 0.402566 0.637010 0.366 Uiso 1 1 calc R U . . . H50C H 0.660682 0.409966 0.663762 0.366 Uiso 1 1 calc R U . . . C17A C 0.424(2) 0.862(4) 0.701(2) 0.12(3) Uiso 0.157(14) 1 d D . P A 2 H17D H 0.380949 0.840549 0.715074 0.175 Uiso 0.157(14) 1 calc R U P A 2 H17E H 0.420444 0.849725 0.672544 0.175 Uiso 0.157(14) 1 calc R U P A 2 H17F H 0.423104 0.913085 0.703928 0.175 Uiso 0.157(14) 1 calc R U P A 2 C18A C 0.5706(15) 0.859(2) 0.6956(12) 0.048(11) Uiso 0.157(14) 1 d D . P A 2 H18D H 0.565180 0.909813 0.690071 0.072 Uiso 0.157(14) 1 calc R U P A 2 H18E H 0.576278 0.833397 0.670560 0.072 Uiso 0.157(14) 1 calc R U P A 2 H18F H 0.616275 0.851382 0.712069 0.072 Uiso 0.157(14) 1 calc R U P A 2 C19A C 0.498(5) 0.843(5) 0.7620(4) 0.11(3) Uiso 0.157(14) 1 d D . P A 2 H19D H 0.546344 0.825398 0.773400 0.166 Uiso 0.1565 1 calc . U P A 2 H19E H 0.454599 0.817649 0.773299 0.166 Uiso 0.1565 1 calc . U P A 2 H19F H 0.493247 0.893834 0.767944 0.166 Uiso 0.1565 1 calc . U P A 2 C22A C 0.124(3) 0.436(4) 0.748(2) 0.09(2) Uiso 0.157(14) 1 d D . P A 2 H22D H 0.127677 0.482461 0.735535 0.138 Uiso 0.157(14) 1 calc R U P A 2 H22E H 0.134593 0.440347 0.776503 0.138 Uiso 0.157(14) 1 calc R U P A 2 H22F H 0.072074 0.416840 0.744263 0.138 Uiso 0.157(14) 1 calc R U P A 2 C23A C 0.1362(19) 0.343(2) 0.7000(11) 0.032(10) Uiso 0.157(14) 1 d D . P A 2 H23D H 0.092927 0.320335 0.713685 0.048 Uiso 0.157(14) 1 calc R U P A 2 H23E H 0.169155 0.306545 0.688200 0.048 Uiso 0.157(14) 1 calc R U P A 2 H23F H 0.116448 0.373988 0.679084 0.048 Uiso 0.157(14) 1 calc R U P A 2 C21A C 0.186(5) 0.350(5) 0.7696(15) 0.05(2) Uiso 0.157(14) 1 d D . P A 2 H21D H 0.140120 0.320992 0.773361 0.082 Uiso 0.157(14) 1 calc R U P A 2 H21E H 0.189235 0.385700 0.790495 0.082 Uiso 0.157(14) 1 calc R U P A 2 H21F H 0.232095 0.319673 0.770702 0.082 Uiso 0.157(14) 1 calc R U P A 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 0.0493(4) 0.0510(5) 0.0573(4) 0.0004(3) -0.0037(3) -0.0107(3) Cl2 0.0466(8) 0.0421(9) 0.0549(9) -0.0014(7) 0.0036(6) -0.0002(6) P03 0.0381(7) 0.0461(10) 0.0506(9) -0.0028(7) 0.0029(6) -0.0033(7) P004 0.0434(8) 0.0471(10) 0.0552(10) -0.0042(8) -0.0020(6) -0.0045(7) Cl1 0.0908(13) 0.0824(15) 0.0590(11) -0.0153(9) 0.0173(9) -0.0243(11) O1 0.035(2) 0.047(3) 0.055(2) -0.0040(19) 0.0059(16) -0.0049(17) N3 0.052(3) 0.042(3) 0.058(3) -0.003(3) -0.011(2) -0.006(2) N4 0.050(3) 0.045(3) 0.064(3) -0.004(3) -0.003(2) -0.004(2) N1 0.047(3) 0.049(3) 0.053(3) 0.000(3) 0.004(2) -0.001(2) N2 0.045(3) 0.053(4) 0.060(3) 0.000(3) 0.013(2) -0.004(2) C1 0.035(3) 0.045(4) 0.051(3) -0.005(3) -0.004(2) -0.003(3) C2 0.034(3) 0.052(4) 0.051(3) -0.005(3) -0.002(2) 0.000(3) C3 0.041(3) 0.053(4) 0.053(4) 0.000(3) -0.007(3) -0.004(3) C24 0.035(3) 0.054(4) 0.053(4) -0.008(3) 0.000(2) -0.007(3) C4 0.040(3) 0.047(4) 0.069(4) -0.008(3) -0.008(3) 0.000(3) C33 0.047(3) 0.050(4) 0.058(4) -0.001(3) 0.000(3) -0.005(3) C13 0.035(3) 0.051(4) 0.052(4) 0.004(3) -0.003(2) -0.005(3) C6 0.036(3) 0.058(5) 0.049(3) -0.005(3) 0.002(2) 0.003(3) C12 0.044(3) 0.048(4) 0.052(4) 0.008(3) -0.003(3) -0.002(3) C8 0.037(3) 0.065(5) 0.051(4) 0.000(3) 0.000(2) -0.005(3) C11 0.050(4) 0.060(5) 0.056(4) 0.017(3) -0.004(3) -0.013(3) C7 0.038(3) 0.068(5) 0.052(4) -0.003(3) 0.006(3) 0.002(3) C5 0.046(3) 0.056(5) 0.064(4) -0.015(3) -0.002(3) 0.011(3) C9 0.040(3) 0.080(6) 0.062(4) 0.014(4) 0.006(3) 0.003(3) C36 0.055(4) 0.047(4) 0.064(4) 0.001(3) -0.011(3) -0.009(3) C10 0.040(3) 0.075(5) 0.060(4) 0.013(4) -0.006(3) -0.015(3) C27 0.043(3) 0.063(5) 0.069(4) 0.004(4) 0.010(3) 0.004(3) C39 0.051(4) 0.057(5) 0.067(4) 0.002(3) -0.003(3) 0.000(3) C34 0.060(4) 0.055(5) 0.065(4) -0.008(3) -0.015(3) -0.003(3) C37 0.070(5) 0.067(5) 0.073(5) 0.010(4) -0.021(4) -0.008(4) C16 0.047(4) 0.055(5) 0.078(5) -0.013(4) -0.002(3) 0.006(3) C21 0.042(7) 0.071(9) 0.094(9) 0.024(5) 0.010(5) -0.014(6) C35 0.069(4) 0.060(5) 0.071(5) -0.017(4) -0.011(3) -0.011(4) C32 0.068(5) 0.064(6) 0.102(6) 0.018(4) 0.015(4) 0.015(4) C30 0.048(4) 0.064(5) 0.073(5) 0.010(4) -0.001(3) 0.000(3) C38 0.058(4) 0.075(5) 0.073(5) 0.001(4) -0.008(3) 0.005(4) C14 0.046(4) 0.074(5) 0.086(5) -0.005(4) 0.013(3) 0.011(3) C25 0.060(4) 0.055(5) 0.067(4) 0.005(3) 0.015(3) -0.006(3) C26 0.071(4) 0.059(5) 0.062(4) 0.006(3) 0.018(3) -0.002(4) C15 0.059(4) 0.077(5) 0.054(4) -0.005(4) -0.002(3) -0.006(4) C29 0.066(5) 0.062(5) 0.093(6) -0.002(4) 0.008(4) 0.012(4) C20 0.059(4) 0.084(6) 0.084(5) 0.030(5) 0.002(4) -0.021(4) C28 0.049(4) 0.089(6) 0.095(6) -0.006(5) 0.003(4) 0.004(4) C31 0.087(6) 0.117(8) 0.092(6) 0.015(6) -0.036(5) -0.015(5) C19 0.071(7) 0.077(8) 0.132(9) -0.052(7) 0.024(6) -0.016(6) C40 0.087(6) 0.084(7) 0.183(10) 0.060(7) 0.004(6) 0.010(5) C41 0.086(6) 0.175(12) 0.110(8) 0.026(7) 0.020(5) 0.040(7) C18 0.062(5) 0.064(7) 0.109(9) -0.024(6) 0.001(5) -0.007(4) C17 0.200(15) 0.041(7) 0.126(10) -0.007(6) -0.074(11) 0.014(8) C23 0.135(13) 0.23(2) 0.102(10) 0.008(11) 0.016(9) -0.138(14) C22 0.020(5) 0.176(16) 0.40(3) 0.190(18) 0.001(10) -0.003(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ge1 P03 93.37(6) . . ? Cl1 Ge1 P004 92.28(7) . . ? P03 Ge1 P004 98.08(6) . . ? C24 P03 C2 103.6(3) . . ? C24 P03 Ge1 97.45(18) . . ? C2 P03 Ge1 99.38(18) . . ? C33 P004 C12 101.6(3) . . ? C33 P004 Ge1 96.8(2) . . ? C12 P004 Ge1 100.3(2) . . ? C13 O1 C1 117.6(4) . . ? C33 N3 C34 108.7(5) . . ? C33 N3 C36 128.1(5) . . ? C34 N3 C36 123.0(5) . . ? C33 N4 C35 110.3(5) . . ? C33 N4 C39 126.4(5) . . ? C35 N4 C39 123.3(6) . . ? C24 N1 C26 110.8(5) . . ? C24 N1 C30 126.3(5) . . ? C26 N1 C30 122.5(5) . . ? C25 N2 C24 108.8(5) . . ? C25 N2 C27 124.3(5) . . ? C24 N2 C27 127.0(5) . . ? O1 C1 C6 121.8(5) . . ? O1 C1 C2 114.0(5) . . ? C6 C1 C2 124.2(6) . . ? C3 C2 C1 117.2(5) . . ? C3 C2 P03 130.0(4) . . ? C1 C2 P03 112.2(5) . . ? C2 C3 C4 121.1(6) . . ? N1 C24 N2 105.7(5) . . ? N1 C24 P03 133.9(4) . . ? N2 C24 P03 120.0(5) . . ? C5 C4 C3 117.2(6) . . ? C5 C4 C16 123.0(6) . . ? C3 C4 C16 119.8(5) . . ? N4 C33 N3 106.4(5) . . ? N4 C33 P004 122.7(4) . . ? N3 C33 P004 130.8(5) . . ? O1 C13 C12 114.2(5) . . ? O1 C13 C8 120.7(5) . . ? C12 C13 C8 125.1(5) . . ? C1 C6 C5 115.8(5) . . ? C1 C6 C7 120.0(6) . . ? C5 C6 C7 123.9(5) . . ? C13 C12 C11 116.6(5) . . ? C13 C12 P004 115.7(4) . . ? C11 C12 P004 127.4(5) . . ? C13 C8 C9 114.4(6) . . ? C13 C8 C7 120.8(5) . . ? C9 C8 C7 124.7(5) . . ? C10 C11 C12 121.7(6) . . ? C8 C7 C6 109.3(5) . . ? C8 C7 C14 110.7(5) . . ? C6 C7 C14 110.9(6) . . ? C8 C7 C15 108.0(5) . . ? C6 C7 C15 109.4(5) . . ? C14 C7 C15 108.5(5) . . ? C4 C5 C6 124.3(6) . . ? C10 C9 C8 124.4(6) . . ? N3 C36 C37 109.6(5) . . ? N3 C36 C38 110.4(5) . . ? C37 C36 C38 111.7(5) . . ? C11 C10 C9 117.6(6) . . ? C11 C10 C20 123.1(7) . . ? C9 C10 C20 119.2(6) . . ? N2 C27 C29 110.6(5) . . ? N2 C27 C28 107.9(6) . . ? C29 C27 C28 113.0(5) . . ? C40 C39 C41 111.9(8) . . ? C40 C39 N4 110.2(6) . . ? C41 C39 N4 109.8(6) . . ? C35 C34 N3 108.0(6) . . ? C18A C16 C19A 117(4) . . ? C18A C16 C17A 114(3) . . ? C19A C16 C17A 108(4) . . ? C17 C16 C19 108.4(9) . . ? C17 C16 C18 108.5(8) . . ? C19 C16 C18 104.7(7) . . ? C18A C16 C4 113.0(17) . . ? C19A C16 C4 107(3) . . ? C17A C16 C4 96(3) . . ? C17 C16 C4 111.1(6) . . ? C19 C16 C4 113.5(6) . . ? C18 C16 C4 110.4(5) . . ? C34 C35 N4 106.7(6) . . ? N1 C30 C32 109.7(5) . . ? N1 C30 C31 109.2(6) . . ? C32 C30 C31 111.3(6) . . ? C26 C25 N2 107.8(6) . . ? C25 C26 N1 106.9(6) . . ? C23A C20 C21A 111(4) . . ? C23A C20 C22A 104(3) . . ? C21A C20 C22A 86(5) . . ? C21 C20 C22 113.9(12) . . ? C21 C20 C23 103.6(11) . . ? C22 C20 C23 110.6(10) . . ? C23A C20 C10 120.6(19) . . ? C21A C20 C10 119(3) . . ? C21 C20 C10 107.2(7) . . ? C22A C20 C10 109(3) . . ? C22 C20 C10 111.3(7) . . ? C23 C20 C10 109.9(7) . . ? C42 O2 C42 142(2) 2_565 . ? N5 C48 C47 177.4(14) . . ? C46 C46 C45 116.1(14) 2_655 . ? O2 C42 C43 107.3(15) . . ? C46 C45 C44 108.4(15) . . ? N6 C49 C50 138(2) . . ? 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 Cl1 2.303(2) . ? Ge1 P03 2.4601(16) . ? Ge1 P004 2.4633(19) . ? P03 C24 1.830(6) . ? P03 C2 1.845(6) . ? P004 C33 1.839(6) . ? P004 C12 1.839(6) . ? O1 C13 1.380(6) . ? O1 C1 1.384(7) . ? N3 C33 1.372(7) . ? N3 C34 1.374(8) . ? N3 C36 1.479(8) . ? N4 C33 1.338(8) . ? N4 C35 1.379(8) . ? N4 C39 1.501(8) . ? N1 C24 1.345(7) . ? N1 C26 1.371(7) . ? N1 C30 1.498(8) . ? N2 C25 1.371(8) . ? N2 C24 1.391(7) . ? N2 C27 1.469(8) . ? C1 C6 1.387(8) . ? C1 C2 1.403(8) . ? C2 C3 1.389(8) . ? C3 C4 1.436(8) . ? C4 C5 1.379(9) . ? C4 C16 1.546(9) . ? C13 C12 1.381(8) . ? C13 C8 1.398(8) . ? C6 C5 1.389(9) . ? C6 C7 1.530(8) . ? C12 C11 1.422(8) . ? C8 C9 1.402(8) . ? C8 C7 1.521(9) . ? C11 C10 1.385(9) . ? C7 C14 1.537(8) . ? C7 C15 1.547(8) . ? C9 C10 1.391(10) . ? C36 C37 1.521(9) . ? C36 C38 1.526(8) . ? C10 C20 1.536(8) . ? C27 C29 1.491(9) . ? C27 C28 1.542(9) . ? C39 C40 1.478(11) . ? C39 C41 1.497(10) . ? C34 C35 1.350(9) . ? C16 C18A 1.520(5) . ? C16 C19A 1.520(5) . ? C16 C17A 1.522(5) . ? C16 C17 1.523(5) . ? C16 C19 1.524(5) . ? C16 C18 1.527(5) . ? C21 C20 1.522(5) . ? C32 C30 1.513(10) . ? C30 C31 1.539(10) . ? C25 C26 1.363(9) . ? C20 C23A 1.518(5) . ? C20 C21A 1.520(5) . ? C20 C22A 1.522(5) . ? C20 C22 1.523(5) . ? C20 C23 1.523(5) . ? O2 C42 1.45(2) 2_565 ? O2 C42 1.45(2) . ? C48 N5 1.094(15) . ? C48 C47 1.361(14) . ? C46 C46 1.366(17) 2_655 ? C46 C45 1.507(5) . ? C43 C42 1.508(5) . ? C45 C44 1.525(5) . ? C49 N6 1.108(5) . ? C49 C50 1.554(19) . ?