#------------------------------------------------------------------------------ #$Date: 2019-08-14 03:06:28 +0300 (Wed, 14 Aug 2019) $ #$Revision: 217510 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/39/7123983.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_7123983 loop_ _publ_author_name 'Ho, Luong Phong' 'Zaretzke, Marc-Kevin' 'Bannenberg, Thomas' 'Tamm, Matthias' _publ_section_title ; Heteroleptic diphosphenes and arsaphosphenes bearing neutral and anionic N-heterocyclic carbenes ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC05739K _journal_year 2019 _chemical_formula_moiety 'C72 H71 B F15 N4 P2, 0.5(C6 H5 Cl), 0.5(C6 H5 Cl)' _chemical_formula_sum 'C78 H76 B Cl5 F15 Ga N4 P2' _chemical_formula_weight 1674.14 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-07-23 deposited with the CCDC. 2019-08-13 downloaded from the CCDC. ; _cell_angle_alpha 83.1200(10) _cell_angle_beta 89.6020(10) _cell_angle_gamma 72.833(2) _cell_formula_units_Z 2 _cell_length_a 10.6105(2) _cell_length_b 14.4633(2) _cell_length_c 26.9560(4) _cell_measurement_reflns_used 38890 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 75.9300 _cell_measurement_theta_min 3.2820 _cell_volume 3922.23(12) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_publication_material ; WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.) ; _computing_structure_refinement ; SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)' ; _computing_structure_solution ; SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.3543 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 161786 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.209 _diffrn_reflns_theta_min 3.223 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 3.132 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.418 _exptl_crystal_description irregular _exptl_crystal_F_000 1716 _exptl_crystal_size_max 0.329 _exptl_crystal_size_mid 0.237 _exptl_crystal_size_min 0.189 _refine_diff_density_max 0.985 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1080 _refine_ls_number_reflns 16378 _refine_ls_number_restraints 271 _refine_ls_restrained_S_all 1.222 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0554 _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^)+(0.1007P)^2^+2.1653P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1541 _refine_ls_wR_factor_ref 0.1688 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12976 _reflns_number_total 16378 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc05739k3.cif _cod_data_source_block ph13ph _cod_database_code 7123983 _shelx_shelxl_version_number 2014/7 _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 0.426 _shelx_estimated_absorpt_t_max 0.589 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 1.54184 10.6105 14.4633 26.9560 83.120 89.602 72.833 ZERR 2.00 0.0002 0.0002 0.0004 0.001 0.001 0.002 LATT 1 SFAC C H B N F P CL GA UNIT 156 152 2 8 30 4 10 2 MERG 2 DFIX 1.75 0.02 C1B Cl1B DFIX 1.75 0.02 C1A Cl1A SADI C1A C2A C2A C3A C3A C4A C4A C5A C5A C6A C6A C1A SADI C1A C3A C3A C5A C2A C6A C2A C4A C4A C6A C1A C5A SADI CL1A C2A CL1A C6A FLAT CL1A C3A C4A C5A C6A SIMU CL1A > C6A RIGU CL1A > C6A ISOR 0.002 C1A C2A C3A C4A C5A C6A Cl1A SADI C1B C2B C2B C3B C3B C4B C4B C5B C5B C6B C6B C1B SADI C1B C3B C3B C5B C2B C6B C2B C4B C4B C6B C1B C5B SADI CL1B C2B CL1B C6B FLAT CL1B > C6B SIMU CL1B > C6B RIGU CL1B > C6B FMAP 2 PLAN 20 SIZE 0.189 0.237 0.329 ACTA CONF LIST 6 L.S. 10 TEMP -173.00 WGHT 0.100700 2.165300 FVAR 3.35982 0.68074 C1 1 0.257977 0.496904 0.792061 11.00000 0.02848 0.02192 = 0.02326 -0.00578 0.00056 -0.00485 C2 1 0.352411 0.381947 0.857593 11.00000 0.02862 0.02385 = 0.02143 -0.00645 0.00156 -0.00623 C3 1 0.323440 0.474270 0.871513 11.00000 0.03071 0.02444 = 0.02184 -0.00605 0.00040 -0.00646 AFIX 43 H3 2 0.339385 0.488400 0.903998 11.00000 -1.20000 AFIX 0 C4 1 0.298331 0.329663 0.773454 11.00000 0.04251 0.02184 = 0.02125 -0.00666 -0.00209 -0.00566 C5 1 0.407294 0.294648 0.743763 11.00000 0.04368 0.02558 = 0.02468 -0.00764 -0.00084 -0.00079 C6 1 0.390414 0.236466 0.707558 11.00000 0.05804 0.03327 = 0.03153 -0.01634 0.00104 -0.00098 AFIX 43 H6 2 0.461415 0.211109 0.686580 11.00000 -1.20000 AFIX 0 C7 1 0.273923 0.215567 0.701880 11.00000 0.06982 0.03634 = 0.03952 -0.01946 -0.00528 -0.01341 AFIX 43 H7 2 0.264774 0.177217 0.676654 11.00000 -1.20000 AFIX 0 C8 1 0.169048 0.249820 0.732591 11.00000 0.05927 0.03717 = 0.03714 -0.01184 -0.00450 -0.02039 AFIX 43 H8 2 0.089791 0.233217 0.728681 11.00000 -1.20000 AFIX 0 C9 1 0.178649 0.308452 0.769205 11.00000 0.04803 0.02798 = 0.02735 -0.00417 -0.00430 -0.01248 C10 1 0.535351 0.319097 0.748908 11.00000 0.03935 0.04156 = 0.02726 -0.01441 0.00256 0.00062 AFIX 13 H10 2 0.536876 0.343421 0.782029 11.00000 -1.20000 AFIX 0 C11 1 0.546516 0.399198 0.708415 11.00000 0.04574 0.03603 = 0.05985 -0.00911 0.00394 -0.00605 AFIX 137 H11A 2 0.548435 0.376195 0.675588 11.00000 -1.50000 H11B 2 0.627891 0.415789 0.714185 11.00000 -1.50000 H11C 2 0.470400 0.457103 0.709442 11.00000 -1.50000 AFIX 0 C12 1 0.655499 0.229850 0.747639 11.00000 0.04333 0.05175 = 0.03467 0.00345 0.00847 0.00691 AFIX 137 H12A 2 0.641486 0.174432 0.769219 11.00000 -1.50000 H12B 2 0.734039 0.243993 0.759598 11.00000 -1.50000 H12C 2 0.668091 0.213841 0.713285 11.00000 -1.50000 AFIX 0 C13 1 0.059314 0.345667 0.801059 11.00000 0.04207 0.03854 = 0.03479 -0.00665 -0.00118 -0.01782 AFIX 13 H13 2 0.085244 0.382302 0.826438 11.00000 -1.20000 AFIX 0 C14 1 0.013585 0.263173 0.829318 11.00000 0.03895 0.04721 = 0.05708 0.00309 0.00033 -0.01710 AFIX 137 H14A 2 -0.005162 0.222524 0.805455 11.00000 -1.50000 H14B 2 -0.066511 0.291183 0.847335 11.00000 -1.50000 H14C 2 0.083244 0.223166 0.853199 11.00000 -1.50000 AFIX 0 C15 1 -0.057475 0.415734 0.770042 11.00000 0.05102 0.04224 = 0.04298 -0.00590 0.00153 -0.01033 AFIX 137 H15A 2 -0.031353 0.471082 0.753490 11.00000 -1.50000 H15B 2 -0.131060 0.439438 0.791963 11.00000 -1.50000 H15C 2 -0.084966 0.381651 0.744767 11.00000 -1.50000 AFIX 0 C16 1 0.220537 0.645832 0.836628 11.00000 0.03158 0.01987 = 0.02389 -0.00658 0.00211 -0.00475 C17 1 0.086073 0.685177 0.842935 11.00000 0.03240 0.02566 = 0.02697 -0.00799 0.00372 -0.00604 C18 1 0.038760 0.785710 0.845331 11.00000 0.03515 0.02703 = 0.03613 -0.00962 0.00745 -0.00274 AFIX 43 H18 2 -0.053090 0.816068 0.848116 11.00000 -1.20000 AFIX 0 C19 1 0.125677 0.840790 0.843645 11.00000 0.04644 0.02315 = 0.03765 -0.00923 0.00734 -0.00533 AFIX 43 H19 2 0.092421 0.909260 0.844183 11.00000 -1.20000 AFIX 0 C20 1 0.259739 0.798048 0.841198 11.00000 0.04273 0.02633 = 0.03357 -0.00708 0.00458 -0.01230 AFIX 43 H20 2 0.317466 0.837143 0.841912 11.00000 -1.20000 AFIX 0 C21 1 0.312706 0.698353 0.837685 11.00000 0.03322 0.02775 = 0.02573 -0.00687 0.00196 -0.00866 C22 1 -0.007295 0.622865 0.851252 11.00000 0.03196 0.03124 = 0.03863 -0.01171 0.00634 -0.00853 AFIX 13 H22 2 0.043440 0.554412 0.846593 11.00000 -1.20000 AFIX 0 C23 1 -0.053792 0.622676 0.904958 11.00000 0.06535 0.05680 = 0.03867 -0.01108 0.01333 -0.03569 AFIX 137 H23A 2 -0.105370 0.688885 0.910343 11.00000 -1.50000 H23B 2 0.022959 0.600133 0.928105 11.00000 -1.50000 H23C 2 -0.108822 0.578890 0.910912 11.00000 -1.50000 AFIX 0 C24 1 -0.123652 0.655976 0.813895 11.00000 0.03378 0.05415 = 0.04894 -0.01537 0.00325 -0.01388 AFIX 137 H24A 2 -0.173904 0.723607 0.817110 11.00000 -1.50000 H24B 2 -0.180895 0.613994 0.820646 11.00000 -1.50000 H24C 2 -0.091017 0.651630 0.779894 11.00000 -1.50000 AFIX 0 C25 1 0.460454 0.649144 0.838113 11.00000 0.03181 0.03022 = 0.03750 -0.00799 0.00172 -0.00830 AFIX 13 H25 2 0.477620 0.585078 0.859580 11.00000 -1.20000 AFIX 0 C26 1 0.511468 0.626980 0.786439 11.00000 0.03563 0.05633 = 0.04194 -0.02150 0.00617 -0.01148 AFIX 137 H26A 2 0.463164 0.587283 0.772549 11.00000 -1.50000 H26B 2 0.605754 0.591204 0.789247 11.00000 -1.50000 H26C 2 0.498237 0.688224 0.764344 11.00000 -1.50000 AFIX 0 C27 1 0.538568 0.706969 0.861879 11.00000 0.03717 0.05148 = 0.03919 -0.01410 0.00453 -0.01822 AFIX 137 H27A 2 0.536290 0.765689 0.839160 11.00000 -1.50000 H27B 2 0.630276 0.666505 0.868159 11.00000 -1.50000 H27C 2 0.499163 0.725743 0.893539 11.00000 -1.50000 AFIX 0 C28 1 0.516209 0.188564 0.872571 11.00000 0.03523 0.02304 = 0.02100 -0.00409 0.00268 -0.00502 C29 1 0.443300 0.133963 0.853488 11.00000 0.03643 0.02441 = 0.02355 -0.00478 0.00128 -0.00457 C30 1 0.497692 0.043901 0.836887 11.00000 0.04770 0.02539 = 0.02592 -0.00661 0.00261 -0.01014 C31 1 0.631811 0.002747 0.839549 11.00000 0.04987 0.02140 = 0.02852 -0.00694 0.00715 -0.00114 C32 1 0.709911 0.052361 0.858182 11.00000 0.03519 0.02867 = 0.02734 -0.00348 0.00497 0.00053 C33 1 0.651563 0.142723 0.874107 11.00000 0.03578 0.02666 = 0.02656 -0.00601 0.00347 -0.00494 C34 1 0.536891 0.335560 0.926206 11.00000 0.03090 0.02212 = 0.02515 -0.00569 -0.00112 -0.00369 C35 1 0.625077 0.374659 0.898746 11.00000 0.03567 0.03057 = 0.02528 -0.00809 0.00088 -0.00644 C36 1 0.708145 0.420269 0.917311 11.00000 0.03699 0.03464 = 0.03366 -0.00665 0.00229 -0.01297 C37 1 0.707469 0.429781 0.968049 11.00000 0.03869 0.03194 = 0.03677 -0.01102 -0.00651 -0.01045 C38 1 0.622635 0.393485 0.997136 11.00000 0.04393 0.03190 = 0.02388 -0.01122 -0.00270 -0.00637 C39 1 0.539232 0.349733 0.976298 11.00000 0.03599 0.02715 = 0.02624 -0.00748 0.00034 -0.00602 C40 1 0.340202 0.251050 0.939348 11.00000 0.03856 0.02353 = 0.02357 -0.00820 0.00211 -0.00715 C41 1 0.398885 0.173174 0.975987 11.00000 0.04437 0.02620 = 0.02756 -0.00595 0.00497 -0.00635 C42 1 0.331428 0.136836 1.013736 11.00000 0.06393 0.02644 = 0.02709 -0.00367 0.00891 -0.00873 C43 1 0.197422 0.176927 1.016105 11.00000 0.06353 0.03528 = 0.02890 -0.00934 0.01734 -0.02045 C44 1 0.132908 0.253435 0.980797 11.00000 0.04334 0.03762 = 0.03327 -0.01265 0.01035 -0.01450 C45 1 0.205853 0.288629 0.944006 11.00000 0.03656 0.02884 = 0.02543 -0.00775 0.00432 -0.00827 C46 1 0.135814 0.729556 0.658271 11.00000 0.03740 0.02707 = 0.02402 -0.00474 0.00068 -0.00650 C47 1 0.060053 0.848918 0.594888 11.00000 0.05209 0.03218 = 0.02988 -0.00067 -0.00301 -0.00537 AFIX 43 H47 2 0.021595 0.911616 0.576920 11.00000 -1.20000 AFIX 0 C48 1 0.107049 0.764232 0.575345 11.00000 0.05483 0.03560 = 0.02581 -0.00151 -0.00436 -0.00866 AFIX 43 H48 2 0.107582 0.756277 0.540861 11.00000 -1.20000 AFIX 0 C49 1 0.043635 0.898255 0.681282 11.00000 0.05434 0.02598 = 0.02925 -0.00336 0.00579 0.00018 C50 1 0.144271 0.930685 0.699029 11.00000 0.06757 0.02579 = 0.02991 -0.00451 0.00642 -0.01276 C51 1 0.110344 0.997270 0.734029 11.00000 0.09482 0.03030 = 0.03692 -0.00971 0.01129 -0.01754 AFIX 43 H51 2 0.175985 1.021027 0.747171 11.00000 -1.20000 AFIX 0 C52 1 -0.017170 1.028579 0.749549 11.00000 0.09840 0.03253 = 0.04108 -0.01057 0.01653 -0.00576 AFIX 43 H52 2 -0.038060 1.072134 0.774179 11.00000 -1.20000 AFIX 0 C53 1 -0.113642 0.998290 0.730264 11.00000 0.07372 0.04274 = 0.04805 -0.00538 0.02254 0.01134 AFIX 43 H53 2 -0.201299 1.022189 0.741213 11.00000 -1.20000 AFIX 0 C54 1 -0.087224 0.932174 0.694344 11.00000 0.05394 0.04311 = 0.04497 -0.00464 0.00637 0.00325 C55 1 0.283475 0.898900 0.680156 11.00000 0.06639 0.04183 = 0.03624 -0.00971 0.00739 -0.02550 AFIX 13 H55 2 0.302425 0.829526 0.673683 11.00000 -1.20000 AFIX 0 C56 1 0.294803 0.959338 0.630032 11.00000 0.09329 0.07172 = 0.03501 -0.00826 0.00964 -0.04710 AFIX 137 H56A 2 0.233461 0.950919 0.605158 11.00000 -1.50000 H56B 2 0.385230 0.937080 0.618389 11.00000 -1.50000 H56C 2 0.272912 1.028398 0.634713 11.00000 -1.50000 AFIX 0 C57 1 0.389050 0.902549 0.717589 11.00000 0.07785 0.06810 = 0.04352 -0.00756 0.00366 -0.03949 AFIX 137 H57A 2 0.380740 0.970638 0.721352 11.00000 -1.50000 H57B 2 0.476732 0.871413 0.705390 11.00000 -1.50000 H57C 2 0.377326 0.867936 0.750013 11.00000 -1.50000 AFIX 0 C58 1 -0.195774 0.903333 0.669844 11.00000 0.05222 0.07819 = 0.06421 -0.01276 0.00217 -0.00329 AFIX 13 H58 2 -0.166521 0.891047 0.635262 11.00000 -1.20000 AFIX 0 C59 1 -0.212407 0.810254 0.694612 11.00000 0.06656 0.06724 = 0.10745 -0.00145 -0.01066 -0.01322 AFIX 137 H59A 2 -0.133822 0.756351 0.689671 11.00000 -1.50000 H59B 2 -0.290088 0.798950 0.680013 11.00000 -1.50000 H59C 2 -0.224271 0.814136 0.730469 11.00000 -1.50000 AFIX 0 C60 1 -0.325284 0.985334 0.663714 11.00000 0.06355 0.08540 = 0.15117 0.03675 -0.01152 -0.01245 AFIX 137 H60A 2 -0.383560 0.970972 0.639637 11.00000 -1.50000 H60B 2 -0.307799 1.046839 0.651511 11.00000 -1.50000 H60C 2 -0.367884 0.990993 0.696047 11.00000 -1.50000 AFIX 0 C61 1 0.223178 0.592342 0.605343 11.00000 0.05773 0.02988 = 0.02235 -0.00676 0.00012 -0.00470 C62 1 0.148383 0.527012 0.603515 11.00000 0.07911 0.03627 = 0.02681 -0.00596 -0.00492 -0.01571 C63 1 0.216472 0.434968 0.591165 11.00000 0.09602 0.03515 = 0.04107 -0.01212 -0.00580 -0.01633 AFIX 43 H63 2 0.171464 0.387321 0.590182 11.00000 -1.20000 AFIX 0 C64 1 0.348834 0.412219 0.580326 11.00000 0.10048 0.03840 = 0.04626 -0.01675 -0.00898 0.00212 AFIX 43 H64 2 0.392868 0.348942 0.571948 11.00000 -1.20000 AFIX 0 C65 1 0.418757 0.478374 0.581295 11.00000 0.06902 0.05685 = 0.03754 -0.01451 0.00219 0.00875 AFIX 43 H65 2 0.509539 0.460469 0.573462 11.00000 -1.20000 AFIX 0 C66 1 0.355895 0.573165 0.593935 11.00000 0.05818 0.04381 = 0.02590 -0.00686 0.00117 -0.00247 C67 1 0.003043 0.555303 0.612688 11.00000 0.07279 0.05431 = 0.04153 -0.00762 -0.00173 -0.03092 AFIX 13 H67 2 -0.016135 0.605831 0.636237 11.00000 -1.20000 AFIX 0 C68 1 -0.042580 0.469304 0.636769 11.00000 0.10191 0.07277 = 0.04746 -0.00109 -0.01113 -0.05262 AFIX 137 H68A 2 -0.053483 0.429720 0.610970 11.00000 -1.50000 H68B 2 -0.126977 0.494199 0.652821 11.00000 -1.50000 H68C 2 0.023618 0.429139 0.661876 11.00000 -1.50000 AFIX 0 C69 1 -0.078877 0.600613 0.564016 11.00000 0.07642 0.08152 = 0.05633 0.01140 -0.01364 -0.03517 AFIX 137 H69A 2 -0.054095 0.658015 0.549548 11.00000 -1.50000 H69B 2 -0.172955 0.620037 0.571427 11.00000 -1.50000 H69C 2 -0.061619 0.552569 0.540156 11.00000 -1.50000 AFIX 0 C70 1 0.430370 0.647619 0.592796 11.00000 0.05081 0.05968 = 0.03924 -0.00203 0.00577 -0.00943 AFIX 13 H70 2 0.364163 0.711772 0.596424 11.00000 -1.20000 AFIX 0 C71 1 0.530890 0.626248 0.635693 11.00000 0.09241 0.09356 = 0.04223 0.00446 -0.00604 -0.04741 AFIX 137 H71A 2 0.487883 0.617157 0.667429 11.00000 -1.50000 H71B 2 0.567530 0.681018 0.635681 11.00000 -1.50000 H71C 2 0.602111 0.566779 0.631647 11.00000 -1.50000 AFIX 0 C72 1 0.497600 0.659776 0.543029 11.00000 0.07792 0.13208 = 0.04066 0.00456 0.00261 -0.04527 AFIX 137 H72A 2 0.565495 0.598741 0.538665 11.00000 -1.50000 H72B 2 0.538556 0.712285 0.543024 11.00000 -1.50000 H72C 2 0.431786 0.676085 0.515541 11.00000 -1.50000 AFIX 0 B1 3 0.435886 0.287630 0.897908 11.00000 0.03082 0.02325 = 0.02318 -0.00746 0.00070 -0.00463 N1 4 0.306594 0.398823 0.807762 11.00000 0.03043 0.02102 = 0.02043 -0.00693 0.00074 -0.00542 N2 4 0.268791 0.542426 0.832247 11.00000 0.02796 0.02205 = 0.02311 -0.00707 0.00252 -0.00598 N3 4 0.078661 0.826856 0.646129 11.00000 0.04094 0.02809 = 0.02658 -0.00427 0.00168 -0.00425 N4 4 0.154173 0.691273 0.614333 11.00000 0.04614 0.02816 = 0.02145 -0.00490 -0.00085 -0.00804 F1 5 0.311166 0.167636 0.851876 11.00000 0.03519 0.02843 = 0.03316 -0.00841 -0.00171 -0.00670 F2 5 0.419283 -0.004072 0.819727 11.00000 0.05650 0.03150 = 0.04527 -0.01720 0.00021 -0.01457 F3 5 0.686851 -0.085078 0.824044 11.00000 0.05904 0.02477 = 0.04928 -0.01614 0.00995 0.00019 F4 5 0.841510 0.013387 0.860682 11.00000 0.03689 0.03646 = 0.04348 -0.00907 0.00691 0.00332 F5 5 0.737162 0.183345 0.892706 11.00000 0.03167 0.03830 = 0.04944 -0.01657 0.00045 -0.00549 F6 5 0.631643 0.369737 0.848894 11.00000 0.04525 0.04796 = 0.02367 -0.00847 0.00458 -0.02047 F7 5 0.788555 0.455746 0.887317 11.00000 0.05197 0.05770 = 0.04237 -0.01204 0.00679 -0.03180 F8 5 0.785355 0.474609 0.987771 11.00000 0.04963 0.04580 = 0.04639 -0.01551 -0.00665 -0.02115 F9 5 0.618180 0.402676 1.046435 11.00000 0.06075 0.04811 = 0.02654 -0.01577 -0.00306 -0.01897 F10 5 0.456137 0.323122 1.009378 11.00000 0.05061 0.04953 = 0.02475 -0.01337 0.00700 -0.02086 F11 5 0.531179 0.133481 0.977495 11.00000 0.04631 0.03221 = 0.03003 -0.00084 0.00206 0.00144 F12 5 0.395887 0.064631 1.048684 11.00000 0.08258 0.03469 = 0.03294 0.00651 0.01171 -0.00322 F13 5 0.129895 0.143094 1.052512 11.00000 0.07908 0.04532 = 0.04061 -0.00909 0.02944 -0.02635 F14 5 0.001929 0.293231 0.982150 11.00000 0.04113 0.05828 = 0.04842 -0.01332 0.01679 -0.01560 F15 5 0.134031 0.365916 0.912300 11.00000 0.03326 0.04003 = 0.03270 -0.00156 0.00210 -0.00451 P1 6 0.200067 0.540110 0.727462 11.00000 0.04509 0.02408 = 0.02379 -0.00475 -0.00437 -0.00761 P2 6 0.184478 0.685885 0.724040 11.00000 0.04820 0.02527 = 0.02406 -0.00477 -0.00097 -0.00925 PART 1 GA1 8 0.162397 0.777740 0.419718 21.00000 0.05527 0.03487 = 0.02715 -0.00278 -0.00506 -0.00693 CL3 7 0.177907 0.640356 0.467151 21.00000 0.11448 0.03836 = 0.02821 -0.00170 -0.00834 -0.02853 CL1 7 0.075122 0.900612 0.461597 21.00000 0.07837 0.03128 = 0.04125 -0.00073 0.01078 0.00258 CL4 7 0.360265 0.777731 0.400632 21.00000 0.05699 0.07161 = 0.04783 -0.00798 0.00878 -0.00297 CL2 7 0.086111 0.780542 0.347384 21.00000 0.17688 0.10546 = 0.03030 0.01083 -0.02106 -0.08199 PART 2 GA2 8 0.080858 0.774826 0.424538 -21.00000 0.04436 0.03611 = 0.02896 0.00047 -0.00062 -0.01028 CL4' 7 -0.124031 0.790174 0.441118 -21.00000 0.04989 0.05167 = 0.06897 -0.00377 0.01105 -0.00953 CL3' 7 0.202665 0.643699 0.465059 -21.00000 0.05754 0.03065 = 0.04205 -0.00680 -0.00215 0.00868 CL1' 7 0.135022 0.895750 0.451897 -21.00000 0.08571 0.04041 = 0.06377 -0.00319 -0.01474 -0.02375 CL2' 7 0.028191 0.794035 0.357840 -21.00000 0.05776 0.06907 = 0.02795 0.00372 -0.01389 -0.02169 PART -1 CL1A 7 0.230794 0.992068 0.927026 10.50000 0.09479 0.08312 = 0.06782 -0.01836 0.00810 -0.03654 C1A 1 0.094329 0.999552 0.965672 10.50000 0.05585 0.05034 = 0.05458 -0.00613 -0.00749 -0.01202 C2A 1 -0.020224 1.074843 0.957333 10.50000 0.05646 0.05122 = 0.05325 -0.00089 -0.00193 -0.01366 AFIX 43 H2A 2 -0.013730 1.120812 0.929891 10.50000 -1.20000 AFIX 0 C3A 1 -0.146159 1.101999 0.979068 10.50000 0.14004 0.14278 = 0.14293 -0.01390 0.00653 -0.03913 AFIX 43 H3A 2 -0.216759 1.156078 0.965079 10.50000 -1.20000 AFIX 0 C4A 1 -0.158416 1.039355 1.025162 10.50000 0.06527 0.06014 = 0.06026 -0.00757 0.00224 -0.02278 AFIX 43 H4A 2 -0.230498 1.040636 1.046444 10.50000 -1.20000 AFIX 0 C5A 1 -0.029053 0.977581 1.027156 10.50000 0.05247 0.05451 = 0.05371 -0.01247 0.00240 -0.02124 AFIX 43 H5A 2 -0.021447 0.944801 1.060213 10.50000 -1.20000 AFIX 0 C6A 1 0.100400 0.934478 1.008003 10.50000 0.06694 0.06385 = 0.06348 -0.00443 -0.00520 -0.01806 AFIX 43 H6A 2 0.169123 0.878029 1.020847 10.50000 -1.20000 AFIX 0 CL1B 7 -0.279562 0.803893 0.454903 10.50000 0.27654 0.07480 = 0.17022 -0.04040 0.09873 -0.05883 C1B 1 -0.439795 0.927647 0.482396 10.50000 0.14691 0.12495 = 0.09583 0.00985 0.02959 -0.06192 C2B 1 -0.404173 1.002460 0.507666 10.50000 0.11311 0.14175 = 0.10994 -0.01606 0.04536 -0.04338 AFIX 43 H2B 2 -0.313342 0.995777 0.513005 10.50000 -1.20000 AFIX 0 C3B 1 -0.496084 1.080869 0.523706 10.50000 0.11611 0.13341 = 0.11279 -0.01081 0.05251 -0.04134 AFIX 43 H3B 2 -0.464142 1.124744 0.539864 10.50000 -1.20000 AFIX 0 C4B 1 -0.637889 1.102238 0.518018 10.50000 0.12995 0.07851 = 0.10332 -0.02083 0.06046 -0.03433 AFIX 43 H4B 2 -0.698145 1.160694 0.526583 10.50000 -1.20000 AFIX 0 C5B 1 -0.677526 1.031740 0.499420 10.50000 0.13721 0.09837 = 0.06856 -0.01609 0.03574 -0.04756 AFIX 43 H5B 2 -0.768733 1.036544 0.498300 10.50000 -1.20000 AFIX 0 C6B 1 -0.581286 0.948266 0.481039 10.50000 0.15031 0.08947 = 0.08410 -0.04153 0.02920 -0.05730 AFIX 43 H6B 2 -0.615654 0.903368 0.466838 10.50000 -1.20000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0554 for 12976 Fo > 4sig(Fo) and 0.0704 for all 16378 data REM 1080 parameters refined using 271 restraints END WGHT 0.1006 2.1645 REM Highest difference peak 0.985, deepest hole -1.261, 1-sigma level 0.072 Q1 1 -0.1943 1.0517 1.0272 11.00000 0.05 0.99 Q2 1 -0.0390 1.0003 1.0186 11.00000 0.05 0.76 Q3 1 -0.7207 1.1109 0.4986 11.00000 0.05 0.69 Q4 1 -0.2946 0.9362 0.6369 11.00000 0.05 0.62 Q5 1 0.1193 0.5393 0.7307 11.00000 0.05 0.58 Q6 1 0.1170 0.8139 0.4520 11.00000 0.05 0.52 Q7 1 -0.4755 0.9618 0.4891 11.00000 0.05 0.49 Q8 1 0.2627 0.6600 0.7148 11.00000 0.05 0.48 Q9 1 -0.1776 0.7695 0.6700 11.00000 0.05 0.40 Q10 1 0.0660 0.6846 0.4878 11.00000 0.05 0.39 Q11 1 0.0336 0.8660 0.4402 11.00000 0.05 0.37 Q12 1 0.2449 1.0677 0.9308 11.00000 0.05 0.36 Q13 1 0.2650 0.6634 0.8375 11.00000 0.05 0.36 Q14 1 0.3422 0.8253 0.4185 11.00000 0.05 0.36 Q15 1 0.5189 0.7079 0.7749 11.00000 0.05 0.35 Q16 1 0.3433 0.9609 0.9292 11.00000 0.05 0.34 Q17 1 0.5719 0.1740 0.8731 11.00000 0.05 0.34 Q18 1 0.1383 0.9201 0.9997 11.00000 0.05 0.32 Q19 1 0.0652 0.7166 0.8452 11.00000 0.05 0.31 Q20 1 0.4813 0.2374 0.8842 11.00000 0.05 0.30 ; _shelx_res_checksum 11056 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2580(2) 0.49690(16) 0.79206(8) 0.0249(4) Uani 1 1 d . . . . . C2 C 0.3524(2) 0.38195(16) 0.85759(8) 0.0247(4) Uani 1 1 d . . . . . C3 C 0.3234(2) 0.47427(16) 0.87151(8) 0.0258(4) Uani 1 1 d . . . . . H3 H 0.3394 0.4884 0.9040 0.031 Uiso 1 1 calc R U . . . C4 C 0.2983(3) 0.32966(16) 0.77345(8) 0.0290(5) Uani 1 1 d . . . . . C5 C 0.4073(3) 0.29465(17) 0.74376(9) 0.0330(5) Uani 1 1 d . . . . . C6 C 0.3904(3) 0.2365(2) 0.70756(10) 0.0426(6) Uani 1 1 d . . . . . H6 H 0.4614 0.2111 0.6866 0.051 Uiso 1 1 calc R U . . . C7 C 0.2739(4) 0.2156(2) 0.70188(11) 0.0478(7) Uani 1 1 d . . . . . H7 H 0.2648 0.1772 0.6767 0.057 Uiso 1 1 calc R U . . . C8 C 0.1690(3) 0.2498(2) 0.73259(11) 0.0426(6) Uani 1 1 d . . . . . H8 H 0.0898 0.2332 0.7287 0.051 Uiso 1 1 calc R U . . . C9 C 0.1786(3) 0.30845(18) 0.76920(9) 0.0341(5) Uani 1 1 d . . . . . C10 C 0.5354(3) 0.3191(2) 0.74891(9) 0.0379(6) Uani 1 1 d . . . . . H10 H 0.5369 0.3434 0.7820 0.046 Uiso 1 1 calc R U . . . C11 C 0.5465(3) 0.3992(2) 0.70842(13) 0.0483(7) Uani 1 1 d . . . . . H11A H 0.5484 0.3762 0.6756 0.072 Uiso 1 1 calc R U . . . H11B H 0.6279 0.4158 0.7142 0.072 Uiso 1 1 calc R U . . . H11C H 0.4704 0.4571 0.7094 0.072 Uiso 1 1 calc R U . . . C12 C 0.6555(3) 0.2299(2) 0.74764(11) 0.0486(7) Uani 1 1 d . . . . . H12A H 0.6415 0.1744 0.7692 0.073 Uiso 1 1 calc R U . . . H12B H 0.7340 0.2440 0.7596 0.073 Uiso 1 1 calc R U . . . H12C H 0.6681 0.2138 0.7133 0.073 Uiso 1 1 calc R U . . . C13 C 0.0593(3) 0.3457(2) 0.80106(10) 0.0370(5) Uani 1 1 d . . . . . H13 H 0.0852 0.3823 0.8264 0.044 Uiso 1 1 calc R U . . . C14 C 0.0136(3) 0.2632(2) 0.82932(13) 0.0476(7) Uani 1 1 d . . . . . H14A H -0.0052 0.2225 0.8055 0.071 Uiso 1 1 calc R U . . . H14B H -0.0665 0.2912 0.8473 0.071 Uiso 1 1 calc R U . . . H14C H 0.0832 0.2232 0.8532 0.071 Uiso 1 1 calc R U . . . C15 C -0.0575(3) 0.4157(2) 0.77004(12) 0.0461(7) Uani 1 1 d . . . . . H15A H -0.0314 0.4711 0.7535 0.069 Uiso 1 1 calc R U . . . H15B H -0.1311 0.4394 0.7920 0.069 Uiso 1 1 calc R U . . . H15C H -0.0850 0.3817 0.7448 0.069 Uiso 1 1 calc R U . . . C16 C 0.2205(2) 0.64583(15) 0.83663(8) 0.0254(4) Uani 1 1 d . . . . . C17 C 0.0861(2) 0.68518(17) 0.84294(9) 0.0285(5) Uani 1 1 d . . . . . C18 C 0.0388(3) 0.78571(18) 0.84533(10) 0.0337(5) Uani 1 1 d . . . . . H18 H -0.0531 0.8161 0.8481 0.040 Uiso 1 1 calc R U . . . C19 C 0.1257(3) 0.84079(18) 0.84365(10) 0.0364(5) Uani 1 1 d . . . . . H19 H 0.0924 0.9093 0.8442 0.044 Uiso 1 1 calc R U . . . C20 C 0.2597(3) 0.79805(18) 0.84120(9) 0.0335(5) Uani 1 1 d . . . . . H20 H 0.3175 0.8371 0.8419 0.040 Uiso 1 1 calc R U . . . C21 C 0.3127(2) 0.69835(17) 0.83768(8) 0.0287(5) Uani 1 1 d . . . . . C22 C -0.0073(3) 0.62286(18) 0.85125(10) 0.0335(5) Uani 1 1 d . . . . . H22 H 0.0434 0.5544 0.8466 0.040 Uiso 1 1 calc R U . . . C23 C -0.0538(4) 0.6227(3) 0.90496(11) 0.0494(7) Uani 1 1 d . . . . . H23A H -0.1054 0.6889 0.9103 0.074 Uiso 1 1 calc R U . . . H23B H 0.0230 0.6001 0.9281 0.074 Uiso 1 1 calc R U . . . H23C H -0.1088 0.5789 0.9109 0.074 Uiso 1 1 calc R U . . . C24 C -0.1237(3) 0.6560(2) 0.81389(12) 0.0447(6) Uani 1 1 d . . . . . H24A H -0.1739 0.7236 0.8171 0.067 Uiso 1 1 calc R U . . . H24B H -0.1809 0.6140 0.8206 0.067 Uiso 1 1 calc R U . . . H24C H -0.0910 0.6516 0.7799 0.067 Uiso 1 1 calc R U . . . C25 C 0.4605(3) 0.64914(18) 0.83811(10) 0.0330(5) Uani 1 1 d . . . . . H25 H 0.4776 0.5851 0.8596 0.040 Uiso 1 1 calc R U . . . C26 C 0.5115(3) 0.6270(2) 0.78644(11) 0.0438(6) Uani 1 1 d . . . . . H26A H 0.4632 0.5873 0.7725 0.066 Uiso 1 1 calc R U . . . H26B H 0.6058 0.5912 0.7892 0.066 Uiso 1 1 calc R U . . . H26C H 0.4982 0.6882 0.7643 0.066 Uiso 1 1 calc R U . . . C27 C 0.5386(3) 0.7070(2) 0.86188(11) 0.0408(6) Uani 1 1 d . . . . . H27A H 0.5363 0.7657 0.8392 0.061 Uiso 1 1 calc R U . . . H27B H 0.6303 0.6665 0.8682 0.061 Uiso 1 1 calc R U . . . H27C H 0.4992 0.7257 0.8935 0.061 Uiso 1 1 calc R U . . . C28 C 0.5162(2) 0.18856(16) 0.87257(8) 0.0271(4) Uani 1 1 d . . . . . C29 C 0.4433(3) 0.13396(17) 0.85349(8) 0.0289(5) Uani 1 1 d . . . . . C30 C 0.4977(3) 0.04390(17) 0.83689(9) 0.0329(5) Uani 1 1 d . . . . . C31 C 0.6318(3) 0.00275(17) 0.83955(9) 0.0350(5) Uani 1 1 d . . . . . C32 C 0.7099(3) 0.05236(18) 0.85818(9) 0.0326(5) Uani 1 1 d . . . . . C33 C 0.6516(3) 0.14272(17) 0.87411(9) 0.0304(5) Uani 1 1 d . . . . . C34 C 0.5369(2) 0.33556(16) 0.92621(8) 0.0267(4) Uani 1 1 d . . . . . C35 C 0.6251(3) 0.37466(18) 0.89875(9) 0.0308(5) Uani 1 1 d . . . . . C36 C 0.7081(3) 0.42027(19) 0.91731(10) 0.0344(5) Uani 1 1 d . . . . . C37 C 0.7075(3) 0.42978(19) 0.96805(10) 0.0352(5) Uani 1 1 d . . . . . C38 C 0.6226(3) 0.39348(18) 0.99714(9) 0.0336(5) Uani 1 1 d . . . . . C39 C 0.5392(3) 0.34973(17) 0.97630(9) 0.0302(5) Uani 1 1 d . . . . . C40 C 0.3402(3) 0.25105(16) 0.93935(8) 0.0286(5) Uani 1 1 d . . . . . C41 C 0.3989(3) 0.17317(17) 0.97599(9) 0.0334(5) Uani 1 1 d . . . . . C42 C 0.3314(3) 0.13684(19) 1.01374(10) 0.0402(6) Uani 1 1 d . . . . . C43 C 0.1974(3) 0.1769(2) 1.01610(10) 0.0409(6) Uani 1 1 d . . . . . C44 C 0.1329(3) 0.2534(2) 0.98080(10) 0.0369(5) Uani 1 1 d . . . . . C45 C 0.2059(3) 0.28863(17) 0.94401(9) 0.0302(5) Uani 1 1 d . . . . . C46 C 0.1358(3) 0.72956(17) 0.65827(9) 0.0300(5) Uani 1 1 d . . . . . C47 C 0.0601(3) 0.8489(2) 0.59489(10) 0.0398(6) Uani 1 1 d . . . . . H47 H 0.0216 0.9116 0.5769 0.048 Uiso 1 1 calc R U . . . C48 C 0.1070(3) 0.7642(2) 0.57534(10) 0.0399(6) Uani 1 1 d . . . . . H48 H 0.1076 0.7563 0.5409 0.048 Uiso 1 1 calc R U . . . C49 C 0.0436(3) 0.89826(18) 0.68128(10) 0.0392(6) Uani 1 1 d . . . . . C50 C 0.1443(3) 0.93069(19) 0.69903(10) 0.0413(6) Uani 1 1 d . . . . . C51 C 0.1103(4) 0.9973(2) 0.73403(11) 0.0538(9) Uani 1 1 d . . . . . H51 H 0.1760 1.0210 0.7472 0.065 Uiso 1 1 calc R U . . . C52 C -0.0172(5) 1.0286(2) 0.74955(12) 0.0599(10) Uani 1 1 d . . . . . H52 H -0.0381 1.0721 0.7742 0.072 Uiso 1 1 calc R U . . . C53 C -0.1136(4) 0.9983(3) 0.73026(13) 0.0612(10) Uani 1 1 d . . . . . H53 H -0.2013 1.0222 0.7412 0.073 Uiso 1 1 calc R U . . . C54 C -0.0872(4) 0.9322(2) 0.69434(12) 0.0513(7) Uani 1 1 d . . . . . C55 C 0.2835(4) 0.8989(2) 0.68016(11) 0.0457(7) Uani 1 1 d . . . . . H55 H 0.3024 0.8295 0.6737 0.055 Uiso 1 1 calc R U . . . C56 C 0.2948(5) 0.9593(3) 0.63003(12) 0.0616(10) Uani 1 1 d . . . . . H56A H 0.2335 0.9509 0.6052 0.092 Uiso 1 1 calc R U . . . H56B H 0.3852 0.9371 0.6184 0.092 Uiso 1 1 calc R U . . . H56C H 0.2729 1.0284 0.6347 0.092 Uiso 1 1 calc R U . . . C57 C 0.3891(4) 0.9025(3) 0.71759(13) 0.0592(9) Uani 1 1 d . . . . . H57A H 0.3807 0.9706 0.7214 0.089 Uiso 1 1 calc R U . . . H57B H 0.4767 0.8714 0.7054 0.089 Uiso 1 1 calc R U . . . H57C H 0.3773 0.8679 0.7500 0.089 Uiso 1 1 calc R U . . . C58 C -0.1958(4) 0.9033(3) 0.66984(17) 0.0680(10) Uani 1 1 d . . . . . H58 H -0.1665 0.8910 0.6353 0.082 Uiso 1 1 calc R U . . . C59 C -0.2124(5) 0.8103(4) 0.6946(2) 0.0826(13) Uani 1 1 d . . . . . H59A H -0.1338 0.7564 0.6897 0.124 Uiso 1 1 calc R U . . . H59B H -0.2901 0.7990 0.6800 0.124 Uiso 1 1 calc R U . . . H59C H -0.2243 0.8141 0.7305 0.124 Uiso 1 1 calc R U . . . C60 C -0.3253(5) 0.9853(4) 0.6637(3) 0.106(2) Uani 1 1 d . . . . . H60A H -0.3836 0.9710 0.6396 0.160 Uiso 1 1 calc R U . . . H60B H -0.3078 1.0468 0.6515 0.160 Uiso 1 1 calc R U . . . H60C H -0.3679 0.9910 0.6960 0.160 Uiso 1 1 calc R U . . . C61 C 0.2232(3) 0.59234(19) 0.60534(9) 0.0381(6) Uani 1 1 d . . . . . C62 C 0.1484(4) 0.5270(2) 0.60352(10) 0.0475(7) Uani 1 1 d . . . . . C63 C 0.2165(4) 0.4350(2) 0.59117(12) 0.0574(9) Uani 1 1 d . . . . . H63 H 0.1715 0.3873 0.5902 0.069 Uiso 1 1 calc R U . . . C64 C 0.3488(5) 0.4122(3) 0.58033(13) 0.0656(11) Uani 1 1 d . . . . . H64 H 0.3929 0.3489 0.5719 0.079 Uiso 1 1 calc R U . . . C65 C 0.4188(4) 0.4784(3) 0.58129(12) 0.0597(9) Uani 1 1 d . . . . . H65 H 0.5095 0.4605 0.5735 0.072 Uiso 1 1 calc R U . . . C66 C 0.3559(3) 0.5732(2) 0.59394(10) 0.0452(7) Uani 1 1 d . . . . . C67 C 0.0030(4) 0.5553(3) 0.61269(12) 0.0534(8) Uani 1 1 d . . . . . H67 H -0.0161 0.6058 0.6362 0.064 Uiso 1 1 calc R U . . . C68 C -0.0426(5) 0.4693(3) 0.63677(14) 0.0687(11) Uani 1 1 d . . . . . H68A H -0.0535 0.4297 0.6110 0.103 Uiso 1 1 calc R U . . . H68B H -0.1270 0.4942 0.6528 0.103 Uiso 1 1 calc R U . . . H68C H 0.0236 0.4291 0.6619 0.103 Uiso 1 1 calc R U . . . C69 C -0.0789(5) 0.6006(3) 0.56402(15) 0.0705(11) Uani 1 1 d . . . . . H69A H -0.0541 0.6580 0.5495 0.106 Uiso 1 1 calc R U . . . H69B H -0.1730 0.6200 0.5714 0.106 Uiso 1 1 calc R U . . . H69C H -0.0616 0.5526 0.5402 0.106 Uiso 1 1 calc R U . . . C70 C 0.4304(3) 0.6476(3) 0.59280(12) 0.0518(7) Uani 1 1 d . . . . . H70 H 0.3642 0.7118 0.5964 0.062 Uiso 1 1 calc R U . . . C71 C 0.5309(5) 0.6262(4) 0.63569(14) 0.0728(12) Uani 1 1 d . . . . . H71A H 0.4879 0.6172 0.6674 0.109 Uiso 1 1 calc R U . . . H71B H 0.5675 0.6810 0.6357 0.109 Uiso 1 1 calc R U . . . H71C H 0.6021 0.5668 0.6316 0.109 Uiso 1 1 calc R U . . . C72 C 0.4976(5) 0.6598(5) 0.54303(14) 0.0818(14) Uani 1 1 d . . . . . H72A H 0.5655 0.5987 0.5387 0.123 Uiso 1 1 calc R U . . . H72B H 0.5386 0.7123 0.5430 0.123 Uiso 1 1 calc R U . . . H72C H 0.4318 0.6761 0.5155 0.123 Uiso 1 1 calc R U . . . B1 B 0.4359(3) 0.28763(18) 0.89791(9) 0.0261(5) Uani 1 1 d . . . . . N1 N 0.30659(19) 0.39882(13) 0.80776(7) 0.0241(4) Uani 1 1 d . . . . . N2 N 0.26879(19) 0.54243(13) 0.83225(7) 0.0243(4) Uani 1 1 d . . . . . N3 N 0.0787(2) 0.82686(15) 0.64613(8) 0.0331(4) Uani 1 1 d . . . . . N4 N 0.1542(2) 0.69127(15) 0.61433(7) 0.0324(4) Uani 1 1 d . . . . . F1 F 0.31117(15) 0.16764(10) 0.85188(5) 0.0324(3) Uani 1 1 d . . . . . F2 F 0.41928(18) -0.00407(11) 0.81973(6) 0.0430(4) Uani 1 1 d . . . . . F3 F 0.68685(19) -0.08508(11) 0.82404(7) 0.0462(4) Uani 1 1 d . . . . . F4 F 0.84151(16) 0.01339(12) 0.86068(6) 0.0417(4) Uani 1 1 d . . . . . F5 F 0.73716(15) 0.18334(12) 0.89271(6) 0.0399(3) Uani 1 1 d . . . . . F6 F 0.63164(16) 0.36974(12) 0.84889(5) 0.0372(3) Uani 1 1 d . . . . . F7 F 0.78855(18) 0.45575(14) 0.88732(6) 0.0468(4) Uani 1 1 d . . . . . F8 F 0.78535(18) 0.47461(13) 0.98777(6) 0.0449(4) Uani 1 1 d . . . . . F9 F 0.61818(19) 0.40268(13) 1.04644(6) 0.0435(4) Uani 1 1 d . . . . . F10 F 0.45614(17) 0.32312(12) 1.00938(5) 0.0396(3) Uani 1 1 d . . . . . F11 F 0.53118(17) 0.13348(11) 0.97749(6) 0.0393(3) Uani 1 1 d . . . . . F12 F 0.3959(2) 0.06463(13) 1.04868(6) 0.0541(5) Uani 1 1 d . . . . . F13 F 0.1299(2) 0.14309(13) 1.05251(7) 0.0531(5) Uani 1 1 d . . . . . F14 F 0.00193(18) 0.29323(14) 0.98215(7) 0.0486(4) Uani 1 1 d . . . . . F15 F 0.13403(15) 0.36592(11) 0.91230(6) 0.0370(3) Uani 1 1 d . . . . . P1 P 0.20007(7) 0.54011(4) 0.72746(2) 0.03138(14) Uani 1 1 d . . . . . P2 P 0.18448(7) 0.68589(4) 0.72404(2) 0.03271(15) Uani 1 1 d . . . . . Ga1 Ga 0.16240(10) 0.77774(4) 0.41972(2) 0.0406(2) Uani 0.681(2) 1 d . . P A 1 Cl3 Cl 0.1779(6) 0.6404(4) 0.46715(18) 0.0592(12) Uani 0.681(2) 1 d . . P A 1 Cl1 Cl 0.0751(2) 0.90061(12) 0.46160(6) 0.0548(5) Uani 0.681(2) 1 d . . P A 1 Cl4 Cl 0.36027(14) 0.77773(11) 0.40063(5) 0.0623(4) Uani 0.681(2) 1 d . . P A 1 Cl2 Cl 0.0861(4) 0.7805(2) 0.34738(8) 0.0970(10) Uani 0.681(2) 1 d . . P A 1 Ga2 Ga 0.08086(19) 0.77483(8) 0.42454(4) 0.0372(4) Uani 0.319(2) 1 d . . P A 2 Cl4' Cl -0.1240(3) 0.7902(2) 0.44112(11) 0.0584(7) Uani 0.319(2) 1 d . . P A 2 Cl3' Cl 0.2027(11) 0.6437(7) 0.4651(4) 0.048(2) Uani 0.319(2) 1 d . . P A 2 Cl1' Cl 0.1350(5) 0.8957(3) 0.45190(17) 0.0624(10) Uani 0.319(2) 1 d . . P A 2 Cl2' Cl 0.0282(4) 0.7940(4) 0.35784(15) 0.0517(8) Uani 0.319(2) 1 d . . P A 2 Cl1A Cl 0.2308(3) 0.99207(18) 0.92703(9) 0.0790(6) Uani 0.5 1 d D U P B -1 C1A C 0.0943(8) 0.9996(5) 0.9657(3) 0.0544(15) Uani 0.5 1 d D U P B -1 C2A C -0.0202(6) 1.0748(5) 0.9573(3) 0.0546(15) Uani 0.5 1 d D U P B -1 H2A H -0.0137 1.1208 0.9299 0.066 Uiso 0.5 1 calc R U P B -1 C3A C -0.1462(11) 1.1020(9) 0.9791(5) 0.143(4) Uani 0.5 1 d D U P B -1 H3A H -0.2168 1.1561 0.9651 0.171 Uiso 0.5 1 calc R U P B -1 C4A C -0.1584(8) 1.0394(6) 1.0252(3) 0.0610(17) Uani 0.5 1 d D U P B -1 H4A H -0.2305 1.0406 1.0464 0.073 Uiso 0.5 1 calc R U P B -1 C5A C -0.0291(7) 0.9776(5) 1.0272(3) 0.0519(15) Uani 0.5 1 d D U P B -1 H5A H -0.0214 0.9448 1.0602 0.062 Uiso 0.5 1 calc R U P B -1 C6A C 0.1004(7) 0.9345(6) 1.0080(3) 0.0653(18) Uani 0.5 1 d D U P B -1 H6A H 0.1691 0.8780 1.0208 0.078 Uiso 0.5 1 calc R U P B -1 Cl1B Cl -0.2796(7) 0.8039(3) 0.4549(2) 0.171(2) Uani 0.5 1 d D . P C -1 C1B C -0.4398(12) 0.9276(8) 0.4824(4) 0.120(4) Uani 0.5 1 d D U P D -1 C2B C -0.4042(12) 1.0025(9) 0.5077(5) 0.121(4) Uani 0.5 1 d D U P D -1 H2B H -0.3133 0.9958 0.5130 0.145 Uiso 0.5 1 calc R U P D -1 C3B C -0.4961(12) 1.0809(10) 0.5237(6) 0.120(4) Uani 0.5 1 d D U P D -1 H3B H -0.4641 1.1247 0.5399 0.145 Uiso 0.5 1 calc R U P D -1 C4B C -0.6379(11) 1.1022(8) 0.5180(5) 0.103(3) Uani 0.5 1 d D U P D -1 H4B H -0.6981 1.1607 0.5266 0.123 Uiso 0.5 1 calc R U P D -1 C5B C -0.6775(11) 1.0317(8) 0.4994(4) 0.098(3) Uani 0.5 1 d D U P D -1 H5B H -0.7687 1.0365 0.4983 0.118 Uiso 0.5 1 calc R U P D -1 C6B C -0.5813(11) 0.9483(8) 0.4810(5) 0.101(3) Uani 0.5 1 d D U P D -1 H6B H -0.6157 0.9034 0.4668 0.121 Uiso 0.5 1 calc R U P D -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0285(11) 0.0219(10) 0.0233(10) -0.0058(8) 0.0006(8) -0.0049(8) C2 0.0286(11) 0.0239(10) 0.0214(10) -0.0065(8) 0.0016(8) -0.0062(8) C3 0.0307(11) 0.0244(10) 0.0218(10) -0.0061(8) 0.0004(8) -0.0065(9) C4 0.0425(14) 0.0218(10) 0.0213(10) -0.0067(8) -0.0021(9) -0.0057(9) C5 0.0437(14) 0.0256(11) 0.0247(10) -0.0076(9) -0.0008(10) -0.0008(10) C6 0.0580(18) 0.0333(13) 0.0315(12) -0.0163(10) 0.0010(12) -0.0010(12) C7 0.070(2) 0.0363(14) 0.0395(14) -0.0195(12) -0.0053(14) -0.0134(14) C8 0.0593(18) 0.0372(13) 0.0371(13) -0.0118(11) -0.0045(12) -0.0204(13) C9 0.0480(15) 0.0280(11) 0.0273(11) -0.0042(9) -0.0043(10) -0.0125(10) C10 0.0394(14) 0.0416(14) 0.0273(11) -0.0144(10) 0.0026(10) 0.0006(11) C11 0.0457(16) 0.0360(14) 0.0598(18) -0.0091(13) 0.0039(14) -0.0060(12) C12 0.0433(16) 0.0517(17) 0.0347(13) 0.0035(12) 0.0085(12) 0.0069(13) C13 0.0421(14) 0.0385(13) 0.0348(12) -0.0066(10) -0.0012(11) -0.0178(11) C14 0.0390(15) 0.0472(16) 0.0571(18) 0.0031(13) 0.0003(13) -0.0171(13) C15 0.0510(17) 0.0422(15) 0.0430(15) -0.0059(12) 0.0015(13) -0.0103(13) C16 0.0316(12) 0.0199(10) 0.0239(10) -0.0066(8) 0.0021(8) -0.0048(8) C17 0.0324(12) 0.0257(11) 0.0270(10) -0.0080(8) 0.0037(9) -0.0060(9) C18 0.0351(13) 0.0270(11) 0.0361(12) -0.0096(9) 0.0074(10) -0.0027(10) C19 0.0464(15) 0.0232(11) 0.0376(13) -0.0092(9) 0.0073(11) -0.0053(10) C20 0.0427(14) 0.0263(11) 0.0336(12) -0.0071(9) 0.0046(10) -0.0123(10) C21 0.0332(12) 0.0277(11) 0.0257(10) -0.0069(8) 0.0020(9) -0.0087(9) C22 0.0320(13) 0.0312(12) 0.0386(13) -0.0117(10) 0.0063(10) -0.0085(10) C23 0.065(2) 0.0568(18) 0.0387(14) -0.0111(13) 0.0133(14) -0.0357(16) C24 0.0338(14) 0.0542(17) 0.0489(16) -0.0154(13) 0.0033(12) -0.0139(12) C25 0.0318(13) 0.0302(11) 0.0375(12) -0.0080(10) 0.0017(10) -0.0083(10) C26 0.0356(14) 0.0563(17) 0.0419(14) -0.0215(13) 0.0062(11) -0.0115(12) C27 0.0372(14) 0.0515(16) 0.0392(13) -0.0141(12) 0.0045(11) -0.0182(12) C28 0.0352(12) 0.0230(10) 0.0210(9) -0.0041(8) 0.0027(8) -0.0050(9) C29 0.0364(13) 0.0244(10) 0.0236(10) -0.0048(8) 0.0013(9) -0.0046(9) C30 0.0477(15) 0.0254(11) 0.0259(11) -0.0066(9) 0.0026(10) -0.0101(10) C31 0.0499(15) 0.0214(10) 0.0285(11) -0.0069(9) 0.0072(10) -0.0011(10) C32 0.0352(13) 0.0287(11) 0.0273(11) -0.0035(9) 0.0050(9) 0.0005(10) C33 0.0358(13) 0.0267(11) 0.0266(10) -0.0060(8) 0.0035(9) -0.0049(9) C34 0.0309(12) 0.0221(10) 0.0252(10) -0.0057(8) -0.0011(8) -0.0037(8) C35 0.0357(13) 0.0306(11) 0.0253(11) -0.0081(9) 0.0009(9) -0.0064(10) C36 0.0370(13) 0.0346(12) 0.0337(12) -0.0066(10) 0.0023(10) -0.0130(10) C37 0.0387(14) 0.0319(12) 0.0368(13) -0.0110(10) -0.0065(10) -0.0104(10) C38 0.0439(14) 0.0319(12) 0.0239(11) -0.0112(9) -0.0027(10) -0.0064(10) C39 0.0360(13) 0.0272(11) 0.0262(11) -0.0075(8) 0.0003(9) -0.0060(9) C40 0.0386(13) 0.0235(10) 0.0236(10) -0.0082(8) 0.0021(9) -0.0072(9) C41 0.0444(14) 0.0262(11) 0.0276(11) -0.0060(9) 0.0050(10) -0.0064(10) C42 0.0639(19) 0.0264(11) 0.0271(11) -0.0037(9) 0.0089(11) -0.0087(12) C43 0.0635(19) 0.0353(13) 0.0289(12) -0.0093(10) 0.0173(12) -0.0204(13) C44 0.0433(15) 0.0376(13) 0.0333(12) -0.0127(10) 0.0103(11) -0.0145(11) C45 0.0366(13) 0.0288(11) 0.0254(10) -0.0077(9) 0.0043(9) -0.0083(10) C46 0.0374(13) 0.0271(11) 0.0240(10) -0.0047(8) 0.0007(9) -0.0065(9) C47 0.0521(16) 0.0322(12) 0.0299(12) -0.0007(10) -0.0030(11) -0.0054(11) C48 0.0548(17) 0.0356(13) 0.0258(11) -0.0015(10) -0.0044(11) -0.0087(12) C49 0.0543(17) 0.0260(11) 0.0293(12) -0.0034(9) 0.0058(11) 0.0002(11) C50 0.0676(19) 0.0258(11) 0.0299(12) -0.0045(9) 0.0064(12) -0.0128(12) C51 0.095(3) 0.0303(13) 0.0369(14) -0.0097(11) 0.0113(16) -0.0175(15) C52 0.098(3) 0.0325(14) 0.0411(16) -0.0106(12) 0.0165(17) -0.0058(16) C53 0.074(2) 0.0427(16) 0.0480(17) -0.0054(14) 0.0225(17) 0.0113(16) C54 0.0539(18) 0.0431(16) 0.0450(16) -0.0046(13) 0.0064(14) 0.0032(14) C55 0.066(2) 0.0418(15) 0.0362(14) -0.0097(11) 0.0074(13) -0.0255(14) C56 0.093(3) 0.072(2) 0.0350(15) -0.0083(15) 0.0096(16) -0.047(2) C57 0.078(2) 0.068(2) 0.0435(16) -0.0076(15) 0.0037(16) -0.039(2) C58 0.052(2) 0.078(3) 0.064(2) -0.0128(19) 0.0022(17) -0.0033(19) C59 0.067(3) 0.067(3) 0.107(4) -0.001(3) -0.011(3) -0.013(2) C60 0.064(3) 0.085(4) 0.151(6) 0.037(4) -0.012(3) -0.012(3) C61 0.0577(17) 0.0299(12) 0.0223(10) -0.0068(9) 0.0001(10) -0.0047(11) C62 0.079(2) 0.0363(14) 0.0268(12) -0.0060(10) -0.0049(13) -0.0157(14) C63 0.096(3) 0.0352(15) 0.0411(16) -0.0121(12) -0.0058(16) -0.0163(17) C64 0.100(3) 0.0384(16) 0.0463(18) -0.0168(14) -0.0090(18) 0.0021(18) C65 0.069(2) 0.057(2) 0.0375(15) -0.0145(14) 0.0022(15) 0.0087(17) C66 0.0582(18) 0.0438(15) 0.0259(12) -0.0069(11) 0.0012(11) -0.0025(13) C67 0.073(2) 0.0543(18) 0.0415(15) -0.0076(13) -0.0017(15) -0.0309(17) C68 0.102(3) 0.073(2) 0.0475(18) -0.0011(17) -0.0111(19) -0.053(2) C69 0.076(3) 0.082(3) 0.056(2) 0.0114(19) -0.0136(19) -0.035(2) C70 0.0508(18) 0.0597(19) 0.0392(15) -0.0020(13) 0.0058(13) -0.0094(15) C71 0.092(3) 0.094(3) 0.0422(18) 0.0045(18) -0.0060(19) -0.047(3) C72 0.078(3) 0.132(4) 0.0407(18) 0.005(2) 0.0026(18) -0.045(3) B1 0.0308(13) 0.0232(11) 0.0232(11) -0.0075(9) 0.0007(9) -0.0046(9) N1 0.0304(10) 0.0210(8) 0.0204(8) -0.0069(7) 0.0007(7) -0.0054(7) N2 0.0280(9) 0.0221(9) 0.0231(8) -0.0071(7) 0.0025(7) -0.0060(7) N3 0.0409(12) 0.0281(10) 0.0266(10) -0.0043(8) 0.0017(8) -0.0043(8) N4 0.0461(12) 0.0282(10) 0.0214(9) -0.0049(7) -0.0008(8) -0.0080(9) F1 0.0352(8) 0.0284(7) 0.0332(7) -0.0084(5) -0.0017(6) -0.0067(6) F2 0.0565(10) 0.0315(7) 0.0453(9) -0.0172(6) 0.0002(7) -0.0146(7) F3 0.0590(11) 0.0248(7) 0.0493(9) -0.0161(6) 0.0100(8) 0.0002(7) F4 0.0369(8) 0.0365(8) 0.0435(8) -0.0091(6) 0.0069(7) 0.0033(6) F5 0.0317(8) 0.0383(8) 0.0494(9) -0.0166(7) 0.0005(6) -0.0055(6) F6 0.0452(9) 0.0480(9) 0.0237(7) -0.0085(6) 0.0046(6) -0.0205(7) F7 0.0520(10) 0.0577(10) 0.0424(9) -0.0120(7) 0.0068(7) -0.0318(8) F8 0.0496(10) 0.0458(9) 0.0464(9) -0.0155(7) -0.0066(7) -0.0212(8) F9 0.0607(10) 0.0481(9) 0.0265(7) -0.0158(6) -0.0031(7) -0.0190(8) F10 0.0506(9) 0.0495(9) 0.0247(7) -0.0134(6) 0.0070(6) -0.0209(7) F11 0.0463(9) 0.0322(7) 0.0300(7) -0.0008(6) 0.0021(6) 0.0014(6) F12 0.0826(14) 0.0347(8) 0.0329(8) 0.0065(6) 0.0117(8) -0.0032(8) F13 0.0791(13) 0.0453(9) 0.0406(9) -0.0091(7) 0.0294(9) -0.0264(9) F14 0.0411(9) 0.0583(10) 0.0484(9) -0.0133(8) 0.0168(7) -0.0156(8) F15 0.0333(8) 0.0400(8) 0.0327(7) -0.0016(6) 0.0021(6) -0.0045(6) P1 0.0451(4) 0.0241(3) 0.0238(3) -0.0047(2) -0.0044(2) -0.0076(2) P2 0.0482(4) 0.0253(3) 0.0241(3) -0.0048(2) -0.0010(2) -0.0093(3) Ga1 0.0553(6) 0.0349(3) 0.0272(2) -0.00278(18) -0.0051(2) -0.0069(2) Cl3 0.114(4) 0.0384(13) 0.0282(9) -0.0017(8) -0.0083(14) -0.0285(16) Cl1 0.0784(12) 0.0313(5) 0.0413(6) -0.0007(4) 0.0108(7) 0.0026(7) Cl4 0.0570(7) 0.0716(8) 0.0478(6) -0.0080(5) 0.0088(5) -0.0030(6) Cl2 0.177(3) 0.1055(19) 0.0303(9) 0.0108(9) -0.0211(14) -0.082(2) Ga2 0.0444(10) 0.0361(6) 0.0290(5) 0.0005(4) -0.0006(5) -0.0103(5) Cl4' 0.0499(14) 0.0517(13) 0.0690(16) -0.0038(11) 0.0111(12) -0.0095(11) Cl3' 0.058(2) 0.031(3) 0.042(3) -0.007(2) -0.0021(15) 0.009(2) Cl1' 0.086(3) 0.0404(15) 0.064(2) -0.0032(15) -0.015(2) -0.024(2) Cl2' 0.0578(18) 0.0691(17) 0.0279(17) 0.0037(13) -0.0139(12) -0.0217(15) Cl1A 0.0948(15) 0.0831(13) 0.0678(11) -0.0184(10) 0.0081(10) -0.0365(11) C1A 0.056(2) 0.050(2) 0.055(2) -0.0061(16) -0.0075(17) -0.0120(17) C2A 0.056(2) 0.051(2) 0.053(2) -0.0009(16) -0.0019(16) -0.0137(16) C3A 0.140(4) 0.143(5) 0.143(4) -0.014(2) 0.007(2) -0.039(2) C4A 0.065(2) 0.060(2) 0.060(2) -0.0076(17) 0.0022(17) -0.0228(17) C5A 0.052(2) 0.055(2) 0.054(2) -0.0125(17) 0.0024(16) -0.0212(17) C6A 0.067(2) 0.064(2) 0.063(2) -0.0044(17) -0.0052(17) -0.0181(17) Cl1B 0.277(6) 0.0748(19) 0.170(4) -0.040(2) 0.099(4) -0.059(3) C1B 0.147(10) 0.125(9) 0.096(8) 0.010(6) 0.030(8) -0.062(8) C2B 0.113(8) 0.142(10) 0.110(9) -0.016(7) 0.045(7) -0.043(7) C3B 0.116(8) 0.133(9) 0.113(9) -0.011(7) 0.053(7) -0.041(7) C4B 0.130(8) 0.079(6) 0.103(7) -0.021(5) 0.060(7) -0.034(6) C5B 0.137(9) 0.098(6) 0.069(5) -0.016(5) 0.036(6) -0.048(6) C6B 0.150(9) 0.089(7) 0.084(7) -0.042(6) 0.029(6) -0.057(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N2 C1 N1 105.92(18) N2 C1 P1 133.62(17) N1 C1 P1 120.43(16) C3 C2 N1 103.34(19) C3 C2 B1 118.71(19) N1 C2 B1 137.71(19) N2 C3 C2 110.49(19) C9 C4 C5 123.8(2) C9 C4 N1 118.1(2) C5 C4 N1 117.9(2) C4 C5 C6 116.2(3) C4 C5 C10 122.8(2) C6 C5 C10 121.0(2) C7 C6 C5 121.5(3) C6 C7 C8 120.7(2) C7 C8 C9 120.8(3) C8 C9 C4 116.9(3) C8 C9 C13 118.5(3) C4 C9 C13 124.6(2) C5 C10 C11 111.9(2) C5 C10 C12 112.0(3) C11 C10 C12 109.1(2) C9 C13 C15 112.0(2) C9 C13 C14 112.9(2) C15 C13 C14 108.5(2) C17 C16 C21 124.1(2) C17 C16 N2 117.3(2) C21 C16 N2 118.5(2) C16 C17 C18 117.3(2) C16 C17 C22 122.8(2) C18 C17 C22 119.8(2) C19 C18 C17 120.0(2) C20 C19 C18 121.1(2) C19 C20 C21 121.5(2) C20 C21 C16 115.7(2) C20 C21 C25 122.0(2) C16 C21 C25 122.2(2) C17 C22 C24 112.3(2) C17 C22 C23 109.6(2) C24 C22 C23 111.3(2) C21 C25 C26 112.9(2) C21 C25 C27 112.2(2) C26 C25 C27 110.7(2) C33 C28 C29 113.0(2) C33 C28 B1 127.7(2) C29 C28 B1 118.5(2) F1 C29 C30 116.1(2) F1 C29 C28 119.3(2) C30 C29 C28 124.6(2) F2 C30 C31 120.2(2) F2 C30 C29 120.3(2) C31 C30 C29 119.4(2) F3 C31 C30 120.5(2) F3 C31 C32 120.3(2) C30 C31 C32 119.2(2) F4 C32 C31 119.9(2) F4 C32 C33 120.5(2) C31 C32 C33 119.6(2) F5 C33 C32 114.4(2) F5 C33 C28 121.4(2) C32 C33 C28 124.2(2) C39 C34 C35 111.7(2) C39 C34 B1 127.4(2) C35 C34 B1 120.7(2) F6 C35 C36 114.8(2) F6 C35 C34 119.1(2) C36 C35 C34 126.1(2) F7 C36 C35 121.1(2) F7 C36 C37 119.9(2) C35 C36 C37 119.0(2) F8 C37 C38 120.9(2) F8 C37 C36 121.2(3) C38 C37 C36 117.9(2) F9 C38 C37 119.4(2) F9 C38 C39 119.9(2) C37 C38 C39 120.7(2) F10 C39 C38 113.4(2) F10 C39 C34 122.1(2) C38 C39 C34 124.5(2) C45 C40 C41 113.3(2) C45 C40 B1 128.4(2) C41 C40 B1 118.2(2) F11 C41 C42 116.1(2) F11 C41 C40 119.3(2) C42 C41 C40 124.4(3) F12 C42 C43 119.8(2) F12 C42 C41 120.7(3) C43 C42 C41 119.5(3) F13 C43 C42 120.5(3) F13 C43 C44 120.3(3) C42 C43 C44 119.2(2) F14 C44 C43 120.2(2) F14 C44 C45 120.7(3) C43 C44 C45 119.1(3) F15 C45 C40 121.0(2) F15 C45 C44 114.5(2) C40 C45 C44 124.5(2) N4 C46 N3 105.9(2) N4 C46 P2 136.41(19) N3 C46 P2 117.25(17) C48 C47 N3 106.7(2) C47 C48 N4 107.8(2) C54 C49 C50 123.8(3) C54 C49 N3 118.8(3) C50 C49 N3 117.5(3) C49 C50 C51 117.0(3) C49 C50 C55 122.1(2) C51 C50 C55 120.8(3) C52 C51 C50 120.5(4) C53 C52 C51 121.0(3) C52 C53 C54 121.7(3) C49 C54 C53 115.9(4) C49 C54 C58 122.0(3) C53 C54 C58 122.1(3) C50 C55 C57 113.8(3) C50 C55 C56 110.9(3) C57 C55 C56 109.9(3) C59 C58 C54 112.8(4) C59 C58 C60 112.5(4) C54 C58 C60 112.6(4) C66 C61 C62 125.2(3) C66 C61 N4 116.6(3) C62 C61 N4 117.8(3) C63 C62 C61 116.0(3) C63 C62 C67 121.7(3) C61 C62 C67 122.3(3) C64 C63 C62 120.7(4) C65 C64 C63 122.0(3) C64 C65 C66 120.3(4) C61 C66 C65 115.7(3) C61 C66 C70 123.7(3) C65 C66 C70 120.5(3) C62 C67 C68 112.8(3) C62 C67 C69 111.5(3) C68 C67 C69 109.0(3) C66 C70 C71 113.0(3) C66 C70 C72 112.4(3) C71 C70 C72 109.7(3) C40 B1 C28 105.07(18) C40 B1 C2 112.6(2) C28 B1 C2 115.22(18) C40 B1 C34 109.76(18) C28 B1 C34 112.7(2) C2 B1 C34 101.64(17) C1 N1 C2 111.05(17) C1 N1 C4 118.88(18) C2 N1 C4 129.99(19) C1 N2 C3 109.13(18) C1 N2 C16 127.80(19) C3 N2 C16 122.82(18) C46 N3 C47 110.0(2) C46 N3 C49 125.5(2) C47 N3 C49 124.4(2) C46 N4 C48 109.7(2) C46 N4 C61 128.8(2) C48 N4 C61 121.3(2) C1 P1 P2 101.11(7) C46 P2 P1 101.88(8) Cl2 Ga1 Cl4 98.84(10) Cl2 Ga1 Cl1 118.77(12) Cl4 Ga1 Cl1 108.70(9) Cl2 Ga1 Cl3 112.50(16) Cl4 Ga1 Cl3 107.24(16) Cl1 Ga1 Cl3 109.66(13) Cl2' Ga2 Cl3' 127.0(3) Cl2' Ga2 Cl4' 86.42(15) Cl3' Ga2 Cl4' 109.3(4) Cl2' Ga2 Cl1' 115.7(2) Cl3' Ga2 Cl1' 106.8(4) Cl4' Ga2 Cl1' 108.48(18) C2A C1A C6A 116.3(6) C2A C1A Cl1A 121.6(5) C6A C1A Cl1A 121.9(6) C1A C2A C3A 136.5(8) C2A C3A C4A 114.5(8) C5A C4A C3A 96.6(6) C4A C5A C6A 155.7(7) C1A C6A C5A 99.3(6) C6B C1B C2B 109.2(8) C3B C2B C1B 123.2(9) C2B C3B C4B 125.4(9) C5B C4B C3B 114.4(8) C4B C5B C6B 120.9(8) C1B C6B C5B 126.5(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N2 1.355(3) C1 N1 1.373(3) C1 P1 1.824(2) C2 C3 1.376(3) C2 N1 1.400(3) C2 B1 1.665(3) C3 N2 1.360(3) C4 C9 1.400(4) C4 C5 1.404(4) C4 N1 1.462(3) C5 C6 1.407(3) C5 C10 1.513(4) C6 C7 1.370(5) C7 C8 1.389(5) C8 C9 1.399(3) C9 C13 1.524(4) C10 C11 1.524(4) C10 C12 1.527(4) C13 C15 1.527(4) C13 C14 1.536(4) C16 C17 1.389(3) C16 C21 1.407(3) C16 N2 1.450(3) C17 C18 1.401(3) C17 C22 1.523(3) C18 C19 1.383(4) C19 C20 1.378(4) C20 C21 1.399(3) C21 C25 1.518(4) C22 C24 1.523(4) C22 C23 1.526(4) C25 C26 1.526(4) C25 C27 1.530(4) C28 C33 1.391(4) C28 C29 1.397(3) C28 B1 1.659(3) C29 F1 1.341(3) C29 C30 1.386(3) C30 F2 1.346(3) C30 C31 1.370(4) C31 F3 1.347(3) C31 C32 1.377(4) C32 F4 1.341(3) C32 C33 1.389(3) C33 F5 1.347(3) C34 C39 1.391(3) C34 C35 1.395(4) C34 B1 1.670(3) C35 F6 1.354(3) C35 C36 1.375(4) C36 F7 1.340(3) C36 C37 1.391(4) C37 F8 1.338(3) C37 C38 1.368(4) C38 F9 1.350(3) C38 C39 1.386(4) C39 F10 1.352(3) C40 C45 1.378(4) C40 C41 1.400(3) C40 B1 1.649(4) C41 F11 1.349(3) C41 C42 1.381(4) C42 F12 1.341(3) C42 C43 1.372(5) C43 F13 1.341(3) C43 C44 1.381(4) C44 F14 1.340(3) C44 C45 1.394(4) C45 F15 1.356(3) C46 N4 1.356(3) C46 N3 1.358(3) C46 P2 1.833(2) C47 C48 1.348(4) C47 N3 1.382(3) C48 N4 1.378(3) C49 C54 1.387(5) C49 C50 1.395(5) C49 N3 1.451(3) C50 C51 1.398(4) C50 C55 1.515(5) C51 C52 1.374(6) C52 C53 1.355(6) C53 C54 1.411(5) C54 C58 1.516(6) C55 C57 1.529(5) C55 C56 1.543(4) C58 C59 1.487(7) C58 C60 1.522(6) C61 C66 1.392(5) C61 C62 1.407(4) C61 N4 1.451(3) C62 C63 1.393(4) C62 C67 1.501(5) C63 C64 1.382(6) C64 C65 1.375(6) C65 C66 1.418(4) C66 C70 1.510(5) C67 C68 1.536(5) C67 C69 1.543(5) C70 C71 1.519(5) C70 C72 1.531(5) P1 P2 2.0564(8) Ga1 Cl2 2.108(2) Ga1 Cl4 2.1581(18) Ga1 Cl1 2.1874(17) Ga1 Cl3 2.193(6) Ga2 Cl2' 1.851(4) Ga2 Cl3' 2.130(9) Ga2 Cl4' 2.168(3) Ga2 Cl1' 2.200(4) Cl1A C1A 1.763(7) C1A C2A 1.370(9) C1A C6A 1.378(9) C2A C3A 1.420(11) C3A C4A 1.476(12) C4A C5A 1.397(9) C5A C6A 1.450(9) C1B C6B 1.442(12) C1B C2B 1.483(12) C2B C3B 1.372(12) C3B C4B 1.449(12) C4B C5B 1.359(11) C5B C6B 1.468(11) 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 N1 C2 C3 N2 -2.3(3) B1 C2 C3 N2 173.1(2) C9 C4 C5 C6 1.1(4) N1 C4 C5 C6 -173.5(2) C9 C4 C5 C10 179.7(2) N1 C4 C5 C10 5.1(3) C4 C5 C6 C7 0.0(4) C10 C5 C6 C7 -178.6(3) C5 C6 C7 C8 -1.3(5) C6 C7 C8 C9 1.6(5) C7 C8 C9 C4 -0.6(4) C7 C8 C9 C13 178.7(3) C5 C4 C9 C8 -0.8(4) N1 C4 C9 C8 173.8(2) C5 C4 C9 C13 180.0(2) N1 C4 C9 C13 -5.4(4) C4 C5 C10 C11 -100.9(3) C6 C5 C10 C11 77.6(3) C4 C5 C10 C12 136.3(2) C6 C5 C10 C12 -45.2(3) C8 C9 C13 C15 -65.3(3) C4 C9 C13 C15 113.9(3) C8 C9 C13 C14 57.6(3) C4 C9 C13 C14 -123.2(3) C21 C16 C17 C18 6.8(4) N2 C16 C17 C18 -177.7(2) C21 C16 C17 C22 -168.3(2) N2 C16 C17 C22 7.2(3) C16 C17 C18 C19 -2.8(4) C22 C17 C18 C19 172.5(2) C17 C18 C19 C20 -2.1(4) C18 C19 C20 C21 3.4(4) C19 C20 C21 C16 0.3(4) C19 C20 C21 C25 -176.2(2) C17 C16 C21 C20 -5.5(3) N2 C16 C21 C20 179.1(2) C17 C16 C21 C25 171.0(2) N2 C16 C21 C25 -4.4(3) C16 C17 C22 C24 -126.1(3) C18 C17 C22 C24 58.9(3) C16 C17 C22 C23 109.7(3) C18 C17 C22 C23 -65.3(3) C20 C21 C25 C26 -104.3(3) C16 C21 C25 C26 79.4(3) C20 C21 C25 C27 21.7(3) C16 C21 C25 C27 -154.6(2) C33 C28 C29 F1 177.2(2) B1 C28 C29 F1 6.2(3) C33 C28 C29 C30 -0.9(3) B1 C28 C29 C30 -171.8(2) F1 C29 C30 F2 0.9(3) C28 C29 C30 F2 179.0(2) F1 C29 C30 C31 -177.0(2) C28 C29 C30 C31 1.1(4) F2 C30 C31 F3 1.4(4) C29 C30 C31 F3 179.4(2) F2 C30 C31 C32 -178.7(2) C29 C30 C31 C32 -0.7(4) F3 C31 C32 F4 0.4(4) C30 C31 C32 F4 -179.5(2) F3 C31 C32 C33 -179.9(2) C30 C31 C32 C33 0.3(4) F4 C32 C33 F5 -1.8(3) C31 C32 C33 F5 178.5(2) F4 C32 C33 C28 179.6(2) C31 C32 C33 C28 -0.1(4) C29 C28 C33 F5 -178.1(2) B1 C28 C33 F5 -8.2(4) C29 C28 C33 C32 0.4(3) B1 C28 C33 C32 170.4(2) C39 C34 C35 F6 -177.9(2) B1 C34 C35 F6 -2.7(3) C39 C34 C35 C36 1.4(4) B1 C34 C35 C36 176.6(2) F6 C35 C36 F7 -0.3(4) C34 C35 C36 F7 -179.6(2) F6 C35 C36 C37 179.3(2) C34 C35 C36 C37 0.1(4) F7 C36 C37 F8 0.5(4) C35 C36 C37 F8 -179.2(2) F7 C36 C37 C38 179.2(2) C35 C36 C37 C38 -0.4(4) F8 C37 C38 F9 -0.4(4) C36 C37 C38 F9 -179.1(2) F8 C37 C38 C39 178.0(2) C36 C37 C38 C39 -0.7(4) F9 C38 C39 F10 2.2(3) C37 C38 C39 F10 -176.2(2) F9 C38 C39 C34 -179.2(2) C37 C38 C39 C34 2.5(4) C35 C34 C39 F10 175.9(2) B1 C34 C39 F10 1.1(4) C35 C34 C39 C38 -2.6(4) B1 C34 C39 C38 -177.4(2) C45 C40 C41 F11 -176.1(2) B1 C40 C41 F11 2.7(3) C45 C40 C41 C42 -0.6(4) B1 C40 C41 C42 178.1(2) F11 C41 C42 F12 -1.5(4) C40 C41 C42 F12 -177.1(2) F11 C41 C42 C43 176.8(2) C40 C41 C42 C43 1.2(4) F12 C42 C43 F13 -1.4(4) C41 C42 C43 F13 -179.8(2) F12 C42 C43 C44 177.9(2) C41 C42 C43 C44 -0.5(4) F13 C43 C44 F14 -1.2(4) C42 C43 C44 F14 179.5(2) F13 C43 C44 C45 178.6(2) C42 C43 C44 C45 -0.7(4) C41 C40 C45 F15 178.4(2) B1 C40 C45 F15 -0.2(4) C41 C40 C45 C44 -0.7(3) B1 C40 C45 C44 -179.3(2) F14 C44 C45 F15 2.0(3) C43 C44 C45 F15 -177.8(2) F14 C44 C45 C40 -178.9(2) C43 C44 C45 C40 1.3(4) N3 C47 C48 N4 -0.2(4) C54 C49 C50 C51 3.6(4) N3 C49 C50 C51 -178.1(2) C54 C49 C50 C55 -174.1(3) N3 C49 C50 C55 4.1(4) C49 C50 C51 C52 -0.2(4) C55 C50 C51 C52 177.5(3) C50 C51 C52 C53 -2.1(5) C51 C52 C53 C54 1.3(5) C50 C49 C54 C53 -4.3(4) N3 C49 C54 C53 177.4(3) C50 C49 C54 C58 173.1(3) N3 C49 C54 C58 -5.2(5) C52 C53 C54 C49 1.8(5) C52 C53 C54 C58 -175.6(4) C49 C50 C55 C57 -154.2(3) C51 C50 C55 C57 28.2(4) C49 C50 C55 C56 81.2(3) C51 C50 C55 C56 -96.4(3) C49 C54 C58 C59 86.4(5) C53 C54 C58 C59 -96.3(5) C49 C54 C58 C60 -145.1(4) C53 C54 C58 C60 32.2(6) C66 C61 C62 C63 2.7(4) N4 C61 C62 C63 175.4(2) C66 C61 C62 C67 -175.4(3) N4 C61 C62 C67 -2.7(4) C61 C62 C63 C64 -1.6(4) C67 C62 C63 C64 176.6(3) C62 C63 C64 C65 0.1(5) C63 C64 C65 C66 0.4(5) C62 C61 C66 C65 -2.3(4) N4 C61 C66 C65 -175.1(2) C62 C61 C66 C70 175.5(3) N4 C61 C66 C70 2.7(4) C64 C65 C66 C61 0.7(4) C64 C65 C66 C70 -177.2(3) C63 C62 C67 C68 33.4(4) C61 C62 C67 C68 -148.5(3) C63 C62 C67 C69 -89.7(4) C61 C62 C67 C69 88.4(4) C61 C66 C70 C71 109.4(4) C65 C66 C70 C71 -72.9(4) C61 C66 C70 C72 -125.7(4) C65 C66 C70 C72 52.0(4) C45 C40 B1 C28 -126.5(2) C41 C40 B1 C28 55.0(3) C45 C40 B1 C2 -0.3(3) C41 C40 B1 C2 -178.88(19) C45 C40 B1 C34 112.1(3) C41 C40 B1 C34 -66.4(3) C33 C28 B1 C40 -117.2(3) C29 C28 B1 C40 52.2(3) C33 C28 B1 C2 118.2(3) C29 C28 B1 C2 -72.3(3) C33 C28 B1 C34 2.2(3) C29 C28 B1 C34 171.7(2) C3 C2 B1 C40 82.5(3) N1 C2 B1 C40 -104.3(3) C3 C2 B1 C28 -157.1(2) N1 C2 B1 C28 16.2(4) C3 C2 B1 C34 -34.9(3) N1 C2 B1 C34 138.4(3) C39 C34 B1 C40 -3.6(3) C35 C34 B1 C40 -178.0(2) C39 C34 B1 C28 -120.3(2) C35 C34 B1 C28 65.3(3) C39 C34 B1 C2 115.8(2) C35 C34 B1 C2 -58.6(3) N2 C1 N1 C2 -1.9(3) P1 C1 N1 C2 176.56(16) N2 C1 N1 C4 175.1(2) P1 C1 N1 C4 -6.4(3) C3 C2 N1 C1 2.6(3) B1 C2 N1 C1 -171.3(3) C3 C2 N1 C4 -174.0(2) B1 C2 N1 C4 12.0(4) C9 C4 N1 C1 -81.5(3) C5 C4 N1 C1 93.4(3) C9 C4 N1 C2 95.0(3) C5 C4 N1 C2 -90.1(3) N1 C1 N2 C3 0.4(3) P1 C1 N2 C3 -177.8(2) N1 C1 N2 C16 -174.0(2) P1 C1 N2 C16 7.8(4) C2 C3 N2 C1 1.2(3) C2 C3 N2 C16 176.0(2) C17 C16 N2 C1 76.2(3) C21 C16 N2 C1 -108.0(3) C17 C16 N2 C3 -97.5(3) C21 C16 N2 C3 78.2(3) N4 C46 N3 C47 0.7(3) P2 C46 N3 C47 174.1(2) N4 C46 N3 C49 -178.4(3) P2 C46 N3 C49 -5.0(4) C48 C47 N3 C46 -0.4(3) C48 C47 N3 C49 178.8(3) C54 C49 N3 C46 -101.5(3) C50 C49 N3 C46 80.1(3) C54 C49 N3 C47 79.5(4) C50 C49 N3 C47 -98.8(3) N3 C46 N4 C48 -0.8(3) P2 C46 N4 C48 -172.3(2) N3 C46 N4 C61 173.2(3) P2 C46 N4 C61 1.8(5) C47 C48 N4 C46 0.6(3) C47 C48 N4 C61 -174.0(3) C66 C61 N4 C46 -92.8(3) C62 C61 N4 C46 93.9(3) C66 C61 N4 C48 80.6(3) C62 C61 N4 C48 -92.7(3) N2 C1 P1 P2 11.0(3) N1 C1 P1 P2 -167.03(17) N4 C46 P2 P1 -28.7(3) N3 C46 P2 P1 160.56(19) C6A C1A C2A C3A -6.9(15) Cl1A C1A C2A C3A 177.9(10) C1A C2A C3A C4A 6.1(16) C2A C3A C4A C5A 1.0(8) C3A C4A C5A C6A -14.0(17) C2A C1A C6A C5A 0.1(9) Cl1A C1A C6A C5A 175.3(5) C4A C5A C6A C1A 13.6(19) C6B C1B C2B C3B -3.7(14) C1B C2B C3B C4B -1(2) C2B C3B C4B C5B 7(2) C3B C4B C5B C6B -7.5(17) C2B C1B C6B C5B 2.5(15) C4B C5B C6B C1B 3.3(19)