#------------------------------------------------------------------------------ #$Date: 2019-08-14 03:06:28 +0300 (Wed, 14 Aug 2019) $ #$Revision: 217510 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/39/7123981.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_7123981 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 As B F15 N4 P, C7 H8, Cl4 Ga' _chemical_formula_sum 'C79 H79 As B Cl4 F15 Ga N4 P' _chemical_formula_weight 1697.68 _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-2018/3 _audit_update_record ; 2019-07-23 deposited with the CCDC. 2019-08-13 downloaded from the CCDC. ; _cell_angle_alpha 102.619(2) _cell_angle_beta 96.156(2) _cell_angle_gamma 110.132(2) _cell_formula_units_Z 2 _cell_length_a 13.8673(2) _cell_length_b 14.4035(2) _cell_length_c 21.4914(4) _cell_measurement_reflns_used 96986 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.2580 _cell_measurement_theta_min 2.7220 _cell_volume 3854.26(13) _computing_cell_refinement 'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)' _computing_publication_material 'OLEX2 v1.2 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)' _computing_structure_refinement 'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)' _computing_structure_solution 'SHELXT-2014/5 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.867 _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at offset/far, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.867 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 177241 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.867 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.121 _diffrn_reflns_theta_min 2.529 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.165 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018) 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 1.463 _exptl_crystal_description plate _exptl_crystal_F_000 1736 _exptl_crystal_size_max 0.626 _exptl_crystal_size_mid 0.342 _exptl_crystal_size_min 0.161 _refine_diff_density_max 2.650 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1022 _refine_ls_number_reflns 21529 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0419 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+2.7401P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.1166 _reflns_Friedel_coverage 0.000 _reflns_number_gt 18672 _reflns_number_total 21529 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc05739k3.cif _cod_data_source_block ph12ph4 _cod_original_cell_volume 3854.26(12) _cod_database_code 7123981 _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_estimated_absorpt_t_min 0.566 _shelx_estimated_absorpt_t_max 0.852 _shelx_res_file ; TITL ph12ph4_a.res in P-1 ph12ph4.res created by SHELXL-2018/3 at 12:31:42 on 05-Dec-2018 REM Old TITL ph12ph4 in P-1 REM SHELXT solution in P-1: R1 0.116, Rweak 0.008, 0.080 REM 0.000 for 0 systematic absences, Orientation As input REM Formula found by SHELXT: C79 B N5 F15 Cl5 As2 CELL 0.71073 13.8673 14.4035 21.4914 102.619 96.156 110.132 ZERR 2 0.0002 0.0002 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H As B Cl F Ga N P UNIT 158 158 2 2 8 30 2 8 2 L.S. 99 0 0 PLAN 20 SIZE 0.626 0.342 0.161 TEMP -173 CONF list 4 fmap 2 53 acta OMIT -1 -1 8 OMIT 6 0 3 REM REM REM WGHT 0.065000 2.740100 FVAR 2.09007 0.43205 AS1 3 0.504067 0.605413 0.819943 11.00000 0.02296 0.02776 = 0.02041 0.01251 0.00767 0.01226 GA1 7 0.870746 0.227186 0.909358 11.00000 0.02141 0.01830 = 0.02929 0.00348 0.00367 0.00597 CL1 5 0.945199 0.393621 0.934066 11.00000 0.02903 0.01929 = 0.04545 0.00579 0.01199 0.00457 P1 9 0.644616 0.620499 0.781608 11.00000 0.02178 0.02220 = 0.02512 0.01100 0.00945 0.00917 CL2 5 0.702060 0.185086 0.883181 11.00000 0.02190 0.03666 = 0.04471 -0.00041 0.00054 0.00566 CL3 5 0.906995 0.182993 0.996897 11.00000 0.04142 0.04331 = 0.04635 0.02417 0.01308 0.02275 CL4 5 0.934577 0.163235 0.830831 11.00000 0.04146 0.04243 = 0.03807 -0.00491 0.00736 0.02061 F1 6 0.431426 0.680818 0.547431 11.00000 0.05530 0.01761 = 0.02470 0.00698 0.01189 0.01532 F11 6 0.429988 0.934258 0.757713 11.00000 0.04409 0.02641 = 0.02447 0.00200 0.00146 0.01455 F5 6 0.433703 1.009101 0.650016 11.00000 0.04996 0.01840 = 0.03111 0.00578 0.01533 0.01416 F4 6 0.577412 1.093266 0.587591 11.00000 0.05170 0.01749 = 0.03554 0.00858 0.01321 0.00803 F12 6 0.355098 1.056207 0.830827 11.00000 0.07077 0.02468 = 0.03037 0.00578 0.01779 0.01804 F15 6 0.104428 0.781080 0.607742 11.00000 0.03705 0.04658 = 0.03882 0.01346 0.00243 0.01825 F3 6 0.650598 0.976228 0.502734 11.00000 0.05411 0.03230 = 0.04175 0.01756 0.02514 0.01508 F6 6 0.204356 0.541269 0.610381 11.00000 0.05464 0.02086 = 0.03240 0.00770 -0.00740 0.00652 F2 6 0.573518 0.768056 0.483878 11.00000 0.06623 0.03164 = 0.03543 0.01142 0.02717 0.02508 F10 6 0.252522 0.824276 0.521597 11.00000 0.04190 0.03734 = 0.03230 0.02090 0.00177 0.01200 F9 6 0.128818 0.696512 0.410589 11.00000 0.04963 0.06921 = 0.02247 0.01853 -0.00097 0.02209 N1 8 0.438438 0.689693 0.709486 11.00000 0.02553 0.01400 = 0.01426 0.00383 0.00339 0.00393 N2 8 0.332662 0.653773 0.775985 11.00000 0.02134 0.01628 = 0.01690 0.00572 0.00264 0.00597 F7 6 0.086346 0.416144 0.498418 11.00000 0.06260 0.02502 = 0.04862 -0.00512 -0.01183 0.00524 F13 6 0.157072 1.045595 0.793258 11.00000 0.07337 0.04086 = 0.06255 0.02100 0.03973 0.03548 F14 6 0.034060 0.903874 0.681095 11.00000 0.04651 0.05969 = 0.06535 0.02988 0.02217 0.03351 F8 6 0.041704 0.490662 0.397406 11.00000 0.05914 0.06034 = 0.02607 -0.00746 -0.01172 0.01326 N3 8 0.675416 0.480505 0.853414 11.00000 0.02134 0.01681 = 0.03628 0.00889 0.00231 0.00594 N4 8 0.792747 0.635566 0.886723 11.00000 0.02082 0.01833 = 0.03796 0.00745 0.00145 0.00763 C1 1 0.423753 0.650470 0.761724 11.00000 0.02220 0.01460 = 0.01517 0.00499 0.00264 0.00526 C4 1 0.522902 0.682267 0.676826 11.00000 0.02939 0.01878 = 0.01478 0.00563 0.00671 0.00792 C20 1 0.259720 0.660280 0.937012 11.00000 0.02467 0.02677 = 0.01993 0.00483 0.00549 0.01011 AFIX 43 H20 2 0.273738 0.707118 0.978656 11.00000 -1.20000 AFIX 0 C2 1 0.356428 0.719823 0.691221 11.00000 0.02936 0.01434 = 0.01614 0.00320 0.00065 0.00647 C17 1 0.214812 0.518030 0.814171 11.00000 0.01877 0.01966 = 0.02360 0.00529 0.00494 0.00640 C46 1 0.701032 0.576036 0.845432 11.00000 0.01956 0.01676 = 0.02875 0.00639 0.00502 0.00653 C3 1 0.291914 0.696202 0.734424 11.00000 0.02568 0.01880 = 0.01872 0.00504 0.00040 0.00825 AFIX 43 H3 2 0.228520 0.707677 0.735234 11.00000 -1.20000 AFIX 0 C21 1 0.308303 0.693890 0.887878 11.00000 0.01945 0.02058 = 0.02051 0.00569 0.00316 0.00798 C16 1 0.284809 0.620152 0.828150 11.00000 0.01797 0.02075 = 0.01860 0.00790 0.00478 0.00816 C62 1 0.496941 0.354293 0.837576 11.00000 0.02598 0.01825 = 0.02684 0.01077 0.00548 0.00850 C18 1 0.168690 0.489285 0.865171 11.00000 0.02259 0.02272 = 0.02949 0.00797 0.00895 0.00409 AFIX 43 H18 2 0.121027 0.420623 0.858378 11.00000 -1.20000 AFIX 0 C10 1 0.626882 0.874322 0.731187 11.00000 0.02997 0.01627 = 0.02480 0.00533 0.00457 0.00422 AFIX 13 H10 2 0.556636 0.879546 0.724664 11.00000 -1.20000 AFIX 0 C19 1 0.191214 0.559138 0.925510 11.00000 0.02401 0.03048 = 0.02546 0.01030 0.01070 0.00865 AFIX 43 H19 2 0.159276 0.537476 0.959542 11.00000 -1.20000 AFIX 0 C5 1 0.615494 0.769813 0.688937 11.00000 0.03091 0.01881 = 0.01954 0.00803 0.00801 0.00659 C61 1 0.589035 0.388905 0.813657 11.00000 0.02282 0.01443 = 0.03329 0.00785 0.00429 0.00573 C49 1 0.852619 0.740014 0.886028 11.00000 0.01813 0.01718 = 0.04088 0.00620 0.00043 0.00510 C9 1 0.509237 0.584751 0.637784 11.00000 0.04135 0.01860 = 0.01682 0.00612 0.00926 0.00876 C63 1 0.415445 0.267114 0.797438 11.00000 0.02515 0.01867 = 0.03369 0.01111 0.00892 0.00615 AFIX 43 H63 2 0.351231 0.241284 0.811549 11.00000 -1.20000 AFIX 0 C33 1 0.467928 0.944257 0.611811 11.00000 0.03779 0.01976 = 0.01950 0.00454 0.00437 0.01175 C28 1 0.426560 0.838923 0.605798 11.00000 0.03636 0.01927 = 0.01564 0.00550 0.00195 0.01069 C64 1 0.426365 0.217374 0.737272 11.00000 0.02911 0.01536 = 0.03606 0.00650 0.00782 0.00436 AFIX 43 H64 2 0.368926 0.159400 0.710067 11.00000 -1.20000 AFIX 0 C41 1 0.331566 0.924061 0.735930 11.00000 0.04476 0.02256 = 0.02534 0.01048 0.01112 0.01509 C66 1 0.604800 0.338305 0.754600 11.00000 0.02961 0.01581 = 0.04862 0.00780 0.01819 0.00662 C50 1 0.840841 0.822253 0.929027 11.00000 0.02014 0.02148 = 0.04585 0.00436 0.00378 0.00687 C22 1 0.186354 0.442156 0.747288 11.00000 0.02490 0.02091 = 0.02374 0.00276 0.00424 0.00378 AFIX 13 H22 2 0.230198 0.477013 0.718817 11.00000 -1.20000 AFIX 0 C54 1 0.918072 0.751979 0.841095 11.00000 0.02027 0.02068 = 0.04096 0.00488 0.00261 0.00693 C29 1 0.467275 0.784486 0.561330 11.00000 0.04299 0.01802 = 0.02018 0.00752 0.00514 0.01290 C65 1 0.520209 0.251405 0.716461 11.00000 0.03674 0.01531 = 0.03951 0.00346 0.01662 0.00673 AFIX 43 H65 2 0.527161 0.215159 0.675690 11.00000 -1.20000 AFIX 0 C25 1 0.379494 0.805693 0.899480 11.00000 0.02911 0.01887 = 0.02031 0.00419 0.00356 0.00552 AFIX 13 H25 2 0.410665 0.812077 0.860016 11.00000 -1.20000 AFIX 0 C40 1 0.274186 0.851743 0.676882 11.00000 0.03895 0.02318 = 0.02254 0.01145 0.00710 0.01422 C58 1 0.933992 0.662332 0.797405 11.00000 0.02453 0.02398 = 0.04441 0.00023 0.00296 0.00750 PART 1 AFIX 13 H58 2 0.866131 0.601995 0.787676 21.00000 -1.20000 AFIX 13 PART 0 PART 2 H58A 2 0.891213 0.596875 0.806530 -21.00000 -1.20000 AFIX 0 PART 0 C67 1 0.488722 0.401606 0.906512 11.00000 0.03440 0.02571 = 0.02388 0.01119 0.00628 0.00841 AFIX 13 H67 2 0.546165 0.471218 0.923070 11.00000 -1.20000 AFIX 0 C13 1 0.407307 0.490890 0.623416 11.00000 0.04611 0.01578 = 0.01890 0.00241 0.00663 0.00533 AFIX 13 H13 2 0.355416 0.512174 0.645568 11.00000 -1.20000 AFIX 0 C6 1 0.696320 0.756204 0.659382 11.00000 0.03515 0.02843 = 0.03032 0.01330 0.01509 0.00856 AFIX 43 H6 2 0.760161 0.813348 0.665861 11.00000 -1.20000 AFIX 0 C34 1 0.240722 0.690087 0.571544 11.00000 0.03501 0.02677 = 0.01982 0.00670 0.00060 0.01074 C42 1 0.294425 0.988721 0.775099 11.00000 0.05545 0.02259 = 0.02921 0.01179 0.01770 0.01682 C68 1 0.384775 0.414168 0.911261 11.00000 0.03919 0.03445 = 0.02791 0.01210 0.01497 0.01155 AFIX 137 H68A 2 0.376825 0.461543 0.886445 11.00000 -1.50000 H68B 2 0.383661 0.441880 0.956961 11.00000 -1.50000 H68C 2 0.327017 0.347155 0.893429 11.00000 -1.50000 AFIX 0 C32 1 0.542275 0.990693 0.578766 11.00000 0.04052 0.01757 = 0.02383 0.00702 0.00465 0.00886 C12 1 0.660515 0.886436 0.803777 11.00000 0.05154 0.02130 = 0.02375 0.00455 0.00633 0.00837 AFIX 137 H12A 2 0.606352 0.835208 0.817661 11.00000 -1.50000 H12B 2 0.669994 0.955578 0.828907 11.00000 -1.50000 H12C 2 0.726696 0.876265 0.811161 11.00000 -1.50000 AFIX 0 C8 1 0.592978 0.576814 0.610140 11.00000 0.05347 0.02517 = 0.02373 0.00758 0.01987 0.01673 AFIX 43 H8 2 0.586705 0.512264 0.583393 11.00000 -1.20000 AFIX 0 C30 1 0.540810 0.827442 0.526755 11.00000 0.04781 0.02552 = 0.02217 0.00812 0.01225 0.01846 C45 1 0.173175 0.848774 0.661422 11.00000 0.04169 0.03112 = 0.03073 0.01653 0.01045 0.01728 C11 1 0.703785 0.963483 0.712073 11.00000 0.03744 0.02095 = 0.03435 0.01032 0.00394 0.00098 AFIX 137 H11A 2 0.775484 0.968184 0.725555 11.00000 -1.50000 H11B 2 0.697257 1.027812 0.733620 11.00000 -1.50000 H11C 2 0.687914 0.951611 0.664793 11.00000 -1.50000 AFIX 0 C14 1 0.361289 0.448644 0.549759 11.00000 0.05970 0.02045 = 0.01840 0.00257 0.00296 0.01321 AFIX 137 H14A 2 0.351153 0.503272 0.532878 11.00000 -1.50000 H14B 2 0.293747 0.391407 0.542155 11.00000 -1.50000 H14C 2 0.409724 0.424409 0.527440 11.00000 -1.50000 AFIX 0 C47 1 0.752072 0.480786 0.900026 11.00000 0.02974 0.02352 = 0.05472 0.01429 -0.00545 0.00992 AFIX 43 H47 2 0.753186 0.423603 0.914852 11.00000 -1.20000 AFIX 0 C51 1 0.898027 0.920333 0.924123 11.00000 0.03251 0.01889 = 0.06028 0.00401 0.00973 0.00996 AFIX 43 H51 2 0.893043 0.978501 0.952403 11.00000 -1.20000 AFIX 0 C7 1 0.685473 0.661076 0.620761 11.00000 0.04686 0.03520 = 0.03138 0.01401 0.02372 0.01824 AFIX 43 H7 2 0.741890 0.653716 0.601478 11.00000 -1.20000 AFIX 0 C48 1 0.825423 0.577517 0.920765 11.00000 0.02752 0.02614 = 0.05501 0.01431 -0.00722 0.00996 AFIX 43 H48 2 0.887678 0.600958 0.952750 11.00000 -1.20000 AFIX 0 C15 1 0.422178 0.403915 0.648547 11.00000 0.06441 0.01822 = 0.02221 0.00537 -0.00034 0.00286 AFIX 137 H15A 2 0.473246 0.382343 0.627552 11.00000 -1.50000 H15B 2 0.355007 0.345459 0.638379 11.00000 -1.50000 H15C 2 0.447781 0.428379 0.695766 11.00000 -1.50000 AFIX 0 C39 1 0.215278 0.723053 0.517585 11.00000 0.03646 0.03471 = 0.02363 0.01071 0.00285 0.01194 C31 1 0.579685 0.932513 0.535746 11.00000 0.04159 0.02585 = 0.02582 0.01182 0.01079 0.01203 C53 1 0.972408 0.851793 0.838372 11.00000 0.02958 0.02558 = 0.05303 0.00981 0.01176 0.00491 AFIX 43 H53 2 1.017471 0.863129 0.808140 11.00000 -1.20000 AFIX 0 C43 1 0.194620 0.983267 0.756346 11.00000 0.06017 0.03075 = 0.04440 0.02063 0.03039 0.02522 C55 1 0.772295 0.807113 0.979309 11.00000 0.02363 0.02826 = 0.05054 0.00262 0.00933 0.00606 AFIX 13 H55 2 0.706865 0.745098 0.958755 11.00000 -1.20000 AFIX 0 C26 1 0.318431 0.875575 0.908480 11.00000 0.04587 0.02721 = 0.05845 0.01644 0.01524 0.01788 AFIX 137 H26A 2 0.262364 0.853730 0.870242 11.00000 -1.50000 H26B 2 0.365674 0.946565 0.913685 11.00000 -1.50000 H26C 2 0.287834 0.871545 0.947321 11.00000 -1.50000 AFIX 0 C35 1 0.192026 0.585254 0.562160 11.00000 0.04358 0.02598 = 0.02282 0.00349 -0.00379 0.01071 C52 1 0.961451 0.934560 0.879210 11.00000 0.03550 0.01909 = 0.06606 0.01061 0.01294 0.00445 AFIX 43 H52 2 0.998165 1.002074 0.876219 11.00000 -1.20000 AFIX 0 C44 1 0.133096 0.912705 0.699588 11.00000 0.04438 0.04195 = 0.04793 0.02723 0.02093 0.02522 C69 1 0.506454 0.334798 0.949908 11.00000 0.05655 0.03979 = 0.03291 0.02049 0.00528 0.01667 AFIX 137 H69A 2 0.453037 0.265030 0.933182 11.00000 -1.50000 H69B 2 0.501467 0.364459 0.994474 11.00000 -1.50000 H69C 2 0.576165 0.332305 0.949739 11.00000 -1.50000 AFIX 0 C38 1 0.150410 0.658816 0.459792 11.00000 0.04266 0.05144 = 0.01966 0.01129 0.00110 0.01845 C56 1 0.740760 0.898790 1.003075 11.00000 0.03401 0.04285 = 0.05512 -0.00098 0.01107 0.01785 AFIX 137 H56A 2 0.802904 0.958650 1.027973 11.00000 -1.50000 H56B 2 0.689388 0.881688 1.030890 11.00000 -1.50000 H56C 2 0.709813 0.914682 0.965568 11.00000 -1.50000 AFIX 0 PART 2 C70' 1 0.714848 0.369563 0.740731 -21.00000 0.03003 0.01879 = 0.02988 0.00376 0.01521 0.00558 AFIX 13 H70' 2 0.762963 0.429226 0.777341 -21.00000 -1.20000 AFIX 0 PART 0 C57 1 0.827624 0.787548 1.038219 11.00000 0.04235 0.03918 = 0.05620 0.01621 0.01766 0.01012 AFIX 137 H57A 2 0.837278 0.722363 1.024502 11.00000 -1.50000 H57B 2 0.784725 0.784128 1.071676 11.00000 -1.50000 H57C 2 0.896109 0.843693 1.055999 11.00000 -1.50000 AFIX 0 C37 1 0.107014 0.554782 0.452960 11.00000 0.04323 0.04636 = 0.02136 -0.00317 -0.00571 0.01139 C23 1 0.209573 0.346937 0.749925 11.00000 0.08115 0.04482 = 0.03703 -0.00724 -0.00763 0.04216 AFIX 137 H23A 2 0.283204 0.367735 0.770311 11.00000 -1.50000 H23B 2 0.196013 0.302716 0.705663 11.00000 -1.50000 H23C 2 0.164437 0.309122 0.775498 11.00000 -1.50000 AFIX 0 C24 1 0.072447 0.410579 0.716527 11.00000 0.03961 0.06417 = 0.03714 -0.01094 -0.01239 0.02527 AFIX 137 H24A 2 0.027747 0.376206 0.743617 11.00000 -1.50000 H24B 2 0.057166 0.363357 0.673075 11.00000 -1.50000 H24C 2 0.058647 0.471722 0.712964 11.00000 -1.50000 AFIX 0 C36 1 0.127679 0.517450 0.504156 11.00000 0.04598 0.02824 = 0.03253 -0.00189 -0.00384 0.00759 C100 1 1.067702 0.908537 0.363873 11.00000 0.05752 0.04683 = 0.09138 0.01175 0.03841 0.01360 AFIX 137 H10A 2 1.032971 0.872762 0.318410 11.00000 -1.50000 H10B 2 1.122872 0.884181 0.376194 11.00000 -1.50000 H10C 2 1.098754 0.982690 0.368962 11.00000 -1.50000 AFIX 0 PART 1 C72 1 0.758937 0.303014 0.733218 21.00000 0.04286 0.10822 = 0.04465 0.03795 0.02081 0.04234 AFIX 137 H72A 2 0.777350 0.312389 0.780104 21.00000 -1.50000 H72B 2 0.822916 0.320591 0.715317 21.00000 -1.50000 H72C 2 0.713321 0.231192 0.711914 21.00000 -1.50000 AFIX 0 PART 0 B1 4 0.326972 0.775702 0.635831 11.00000 0.03446 0.01885 = 0.01738 0.00602 0.00174 0.01030 C27 1 0.469412 0.840431 0.957671 11.00000 0.04571 0.02727 = 0.05059 0.00996 -0.01838 -0.00160 AFIX 137 H27A 2 0.441346 0.840545 0.997628 11.00000 -1.50000 H27B 2 0.518194 0.909938 0.960664 11.00000 -1.50000 H27C 2 0.506401 0.793103 0.952067 11.00000 -1.50000 AFIX 0 C106 1 0.887057 0.892252 0.392288 11.00000 0.07252 0.03395 = 0.06145 0.00858 0.00997 0.01412 AFIX 43 H106 2 0.871966 0.910882 0.353692 11.00000 -1.20000 AFIX 0 C102 1 1.003034 0.858671 0.466148 11.00000 0.05379 0.06115 = 0.06413 0.00323 0.00296 0.02657 AFIX 43 H102 2 1.068550 0.853895 0.478826 11.00000 -1.20000 AFIX 0 C105 1 0.813348 0.871853 0.430889 11.00000 0.04930 0.04565 = 0.06177 0.00543 0.00036 0.01326 AFIX 43 H105 2 0.747848 0.876915 0.418616 11.00000 -1.20000 AFIX 0 C101 1 0.983454 0.885594 0.409771 11.00000 0.06344 0.03379 = 0.07466 -0.00066 0.01893 0.00844 C104 1 0.833217 0.844030 0.487409 11.00000 0.05449 0.05151 = 0.06207 0.00715 0.00653 0.01316 AFIX 43 H104 2 0.781518 0.829269 0.513346 11.00000 -1.20000 AFIX 0 PART 1 C59 1 0.955335 0.677175 0.737783 21.00000 0.04699 0.03776 = 0.03560 0.00440 0.01561 0.01497 AFIX 137 H59A 2 0.903237 0.699139 0.717591 21.00000 -1.50000 H59B 2 0.952360 0.612644 0.709273 21.00000 -1.50000 H59C 2 1.025451 0.730205 0.744456 21.00000 -1.50000 AFIX 0 PART 0 C103 1 0.927340 0.838208 0.505088 11.00000 0.07126 0.06650 = 0.06193 0.00936 -0.00047 0.02897 AFIX 43 H103 2 0.942154 0.820212 0.543979 11.00000 -1.20000 AFIX 0 PART 1 C60 1 1.017237 0.634955 0.837630 21.00000 0.04212 0.04155 = 0.04582 0.00123 0.00800 0.02772 AFIX 137 H60A 2 1.084569 0.693511 0.850221 21.00000 -1.50000 H60B 2 1.025749 0.574878 0.810899 21.00000 -1.50000 H60C 2 0.993156 0.619452 0.876781 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C60' 1 1.050946 0.677472 0.809787 -21.00000 0.03384 0.04670 = 0.06564 -0.00225 0.00243 0.02163 AFIX 137 H60D 2 1.092207 0.738914 0.797763 -21.00000 -1.50000 H60E 2 1.059698 0.617221 0.783478 -21.00000 -1.50000 H60F 2 1.075112 0.685886 0.855973 -21.00000 -1.50000 AFIX 0 C59' 1 0.903552 0.653077 0.720447 -21.00000 0.04376 0.05135 = 0.03142 0.00212 0.00951 0.02134 AFIX 137 H59D 2 0.828675 0.639125 0.708665 -21.00000 -1.50000 H59E 2 0.919087 0.596820 0.694619 -21.00000 -1.50000 H59F 2 0.944558 0.717712 0.711698 -21.00000 -1.50000 AFIX 0 C71' 1 0.712739 0.403742 0.678428 -21.00000 0.04517 0.03514 = 0.05873 0.02351 0.03156 0.02102 AFIX 137 H71A 2 0.664164 0.346436 0.642415 -21.00000 -1.50000 H71B 2 0.783197 0.425211 0.668557 -21.00000 -1.50000 H71C 2 0.689501 0.461543 0.684274 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C71 1 0.683051 0.372405 0.651359 21.00000 0.03194 0.03476 = 0.03246 0.01455 0.01365 0.01371 AFIX 137 H71D 2 0.640452 0.302320 0.624705 21.00000 -1.50000 H71E 2 0.750463 0.396364 0.637691 21.00000 -1.50000 H71F 2 0.646162 0.418035 0.645817 21.00000 -1.50000 AFIX 0 C70 1 0.701442 0.373160 0.721211 21.00000 0.02786 0.02328 = 0.02329 0.00297 0.01056 0.00351 AFIX 13 H70 2 0.747543 0.444936 0.746693 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C72' 1 0.757345 0.283785 0.732469 -21.00000 0.02825 0.03001 = 0.04582 0.00345 0.00686 0.01562 AFIX 137 H72D 2 0.759057 0.261491 0.772374 -21.00000 -1.50000 H72E 2 0.828401 0.309287 0.723818 -21.00000 -1.50000 H72F 2 0.711844 0.225544 0.695915 -21.00000 -1.50000 AFIX 0 HKLF 4 REM ph12ph4_a.res in P-1 REM wR2 = 0.1166, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0419 for 18672 Fo > 4sig(Fo) and 0.0494 for all 21529 data REM 1022 parameters refined using 0 restraints END WGHT 0.0650 2.7405 REM Highest difference peak 2.650, deepest hole -1.151, 1-sigma level 0.077 Q1 1 0.4657 0.5551 0.7970 11.00000 0.05 2.65 Q2 1 0.5364 0.6799 0.8997 11.00000 0.05 1.72 Q3 1 0.8134 0.9212 0.3917 11.00000 0.05 1.47 Q4 1 0.8382 0.2092 0.8782 11.00000 0.05 0.89 Q5 1 0.9739 0.8995 0.3505 11.00000 0.05 0.79 Q6 1 0.9027 0.1979 0.8992 11.00000 0.05 0.71 Q7 1 0.8531 0.8280 0.5404 11.00000 0.05 0.65 Q8 1 0.4649 0.6173 0.7896 11.00000 0.05 0.62 Q9 1 0.8629 0.1438 0.9666 11.00000 0.05 0.58 Q10 1 0.4704 0.6470 0.8274 11.00000 0.05 0.55 Q11 1 1.1176 0.8796 0.4125 11.00000 0.05 0.53 Q12 1 0.1052 0.6329 0.4029 11.00000 0.05 0.51 Q13 1 0.5389 0.6155 0.8637 11.00000 0.05 0.50 Q14 1 0.9112 0.3850 0.9007 11.00000 0.05 0.50 Q15 1 0.5569 0.5952 0.8360 11.00000 0.05 0.49 Q16 1 0.6888 0.1772 0.8485 11.00000 0.05 0.49 Q17 1 0.9001 0.1701 0.8044 11.00000 0.05 0.44 Q18 1 1.0778 0.8812 0.4583 11.00000 0.05 0.42 Q19 1 0.0571 0.3834 0.5214 11.00000 0.05 0.41 Q20 1 0.5599 0.5982 0.8050 11.00000 0.05 0.41 ; _shelx_res_checksum 99076 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 As1 As 0.50407(2) 0.60541(2) 0.81994(2) 0.02171(5) Uani 1 1 d . . . . . Ga1 Ga 0.87075(2) 0.22719(2) 0.90936(2) 0.02405(5) Uani 1 1 d . . . . . Cl1 Cl 0.94520(4) 0.39362(3) 0.93407(3) 0.03267(10) Uani 1 1 d . . . . . P1 P 0.64462(4) 0.62050(3) 0.78161(2) 0.02165(9) Uani 1 1 d . . . . . Cl2 Cl 0.70206(4) 0.18509(4) 0.88318(3) 0.03837(12) Uani 1 1 d . . . . . Cl3 Cl 0.90700(5) 0.18299(4) 0.99690(3) 0.03948(12) Uani 1 1 d . . . . . Cl4 Cl 0.93458(5) 0.16324(5) 0.83083(3) 0.04208(13) Uani 1 1 d . . . . . F1 F 0.43143(11) 0.68082(8) 0.54743(5) 0.0316(3) Uani 1 1 d . . . . . F11 F 0.42999(10) 0.93426(9) 0.75771(6) 0.0326(3) Uani 1 1 d . . . . . F5 F 0.43370(10) 1.00910(8) 0.65002(6) 0.0324(3) Uani 1 1 d . . . . . F4 F 0.57741(11) 1.09327(9) 0.58759(6) 0.0357(3) Uani 1 1 d . . . . . F12 F 0.35510(12) 1.05621(9) 0.83083(6) 0.0416(3) Uani 1 1 d . . . . . F15 F 0.10443(11) 0.78108(11) 0.60774(7) 0.0403(3) Uani 1 1 d . . . . . F3 F 0.65060(12) 0.97623(10) 0.50273(7) 0.0406(3) Uani 1 1 d . . . . . F6 F 0.20436(11) 0.54127(9) 0.61038(6) 0.0394(3) Uani 1 1 d . . . . . F2 F 0.57352(12) 0.76806(10) 0.48388(6) 0.0409(3) Uani 1 1 d . . . . . F10 F 0.25252(10) 0.82428(10) 0.52160(6) 0.0366(3) Uani 1 1 d . . . . . F9 F 0.12882(12) 0.69651(13) 0.41059(6) 0.0469(3) Uani 1 1 d . . . . . N1 N 0.43844(12) 0.68969(10) 0.70949(7) 0.0190(3) Uani 1 1 d . . . . . N2 N 0.33266(11) 0.65377(10) 0.77599(7) 0.0184(3) Uani 1 1 d . . . . . F7 F 0.08635(13) 0.41614(10) 0.49842(8) 0.0530(4) Uani 1 1 d . . . . . F13 F 0.15707(14) 1.04559(11) 0.79326(8) 0.0518(4) Uani 1 1 d . . . . . F14 F 0.03406(12) 0.90387(13) 0.68110(8) 0.0504(4) Uani 1 1 d . . . . . F8 F 0.04170(13) 0.49066(13) 0.39741(7) 0.0560(4) Uani 1 1 d . . . . . N3 N 0.67542(12) 0.48051(11) 0.85341(8) 0.0252(3) Uani 1 1 d . . . . . N4 N 0.79275(12) 0.63557(12) 0.88672(8) 0.0260(3) Uani 1 1 d . . . . . C1 C 0.42375(13) 0.65047(12) 0.76172(8) 0.0177(3) Uani 1 1 d . . . . . C4 C 0.52290(14) 0.68227(13) 0.67683(8) 0.0210(3) Uani 1 1 d . . . . . C20 C 0.25972(14) 0.66028(14) 0.93701(8) 0.0239(3) Uani 1 1 d . . . . . H20 H 0.273738 0.707118 0.978656 0.029 Uiso 1 1 calc R U . . . C2 C 0.35643(14) 0.71982(12) 0.69122(8) 0.0209(3) Uani 1 1 d . . . . . C17 C 0.21481(13) 0.51803(13) 0.81417(8) 0.0210(3) Uani 1 1 d . . . . . C46 C 0.70103(13) 0.57604(13) 0.84543(9) 0.0217(3) Uani 1 1 d . . . . . C3 C 0.29191(14) 0.69620(13) 0.73442(8) 0.0215(3) Uani 1 1 d . . . . . H3 H 0.228520 0.707677 0.735234 0.026 Uiso 1 1 calc R U . . . C21 C 0.30830(13) 0.69389(13) 0.88788(8) 0.0201(3) Uani 1 1 d . . . . . C16 C 0.28481(13) 0.62015(13) 0.82815(8) 0.0184(3) Uani 1 1 d . . . . . C62 C 0.49694(14) 0.35429(13) 0.83758(9) 0.0229(3) Uani 1 1 d . . . . . C18 C 0.16869(14) 0.48929(14) 0.86517(9) 0.0257(3) Uani 1 1 d . . . . . H18 H 0.121027 0.420623 0.858378 0.031 Uiso 1 1 calc R U . . . C10 C 0.62688(15) 0.87432(13) 0.73119(9) 0.0251(3) Uani 1 1 d . . . . . H10 H 0.556636 0.879546 0.724664 0.030 Uiso 1 1 calc R U . . . C19 C 0.19121(15) 0.55914(15) 0.92551(9) 0.0262(4) Uani 1 1 d . . . . . H19 H 0.159276 0.537476 0.959542 0.031 Uiso 1 1 calc R U . . . C5 C 0.61549(15) 0.76981(13) 0.68894(8) 0.0232(3) Uani 1 1 d . . . . . C61 C 0.58903(14) 0.38890(13) 0.81366(9) 0.0238(3) Uani 1 1 d . . . . . C49 C 0.85262(14) 0.74001(13) 0.88603(10) 0.0266(4) Uani 1 1 d . . . . . C9 C 0.50924(16) 0.58475(14) 0.63778(8) 0.0258(4) Uani 1 1 d . . . . . C63 C 0.41545(15) 0.26711(13) 0.79744(10) 0.0255(3) Uani 1 1 d . . . . . H63 H 0.351231 0.241284 0.811549 0.031 Uiso 1 1 calc R U . . . C33 C 0.46793(16) 0.94426(14) 0.61181(9) 0.0257(4) Uani 1 1 d . . . . . C28 C 0.42656(15) 0.83892(13) 0.60580(8) 0.0239(3) Uani 1 1 d . . . . . C64 C 0.42636(15) 0.21737(13) 0.73727(10) 0.0279(4) Uani 1 1 d . . . . . H64 H 0.368926 0.159400 0.710067 0.034 Uiso 1 1 calc R U . . . C41 C 0.33157(17) 0.92406(15) 0.73593(9) 0.0292(4) Uani 1 1 d . . . . . C66 C 0.60480(16) 0.33830(14) 0.75460(11) 0.0312(4) Uani 1 1 d . . . . . C50 C 0.84084(15) 0.82225(14) 0.92903(11) 0.0305(4) Uani 1 1 d . . . . . C22 C 0.18635(14) 0.44216(14) 0.74729(9) 0.0251(3) Uani 1 1 d . . . . . H22 H 0.230198 0.477013 0.718817 0.030 Uiso 1 1 calc R U . . . C54 C 0.91807(14) 0.75198(14) 0.84109(10) 0.0284(4) Uani 1 1 d . . . . . C29 C 0.46727(17) 0.78449(13) 0.56133(9) 0.0264(4) Uani 1 1 d . . . . . C65 C 0.52021(17) 0.25140(14) 0.71646(11) 0.0313(4) Uani 1 1 d . . . . . H65 H 0.527161 0.215159 0.675690 0.038 Uiso 1 1 calc R U . . . C25 C 0.37949(15) 0.80569(13) 0.89948(9) 0.0241(3) Uani 1 1 d . . . . . H25 H 0.410665 0.812077 0.860016 0.029 Uiso 1 1 calc R U . . . C40 C 0.27419(16) 0.85174(14) 0.67688(9) 0.0266(4) Uani 1 1 d . . . . . C58 C 0.93399(16) 0.66233(15) 0.79741(11) 0.0333(4) Uani 1 1 d . . . . . H58 H 0.866131 0.601995 0.787676 0.040 Uiso 0.432(10) 1 calc R U P A 1 H58A H 0.891213 0.596875 0.806530 0.040 Uiso 0.568(10) 1 calc R U P A 2 C67 C 0.48872(16) 0.40161(15) 0.90651(9) 0.0280(4) Uani 1 1 d . . . . . H67 H 0.546165 0.471218 0.923070 0.034 Uiso 1 1 calc R U . . . C13 C 0.40731(17) 0.49089(13) 0.62342(9) 0.0291(4) Uani 1 1 d . . . . . H13 H 0.355416 0.512174 0.645568 0.035 Uiso 1 1 calc R U . . . C6 C 0.69632(17) 0.75620(16) 0.65938(10) 0.0307(4) Uani 1 1 d . . . . . H6 H 0.760161 0.813348 0.665861 0.037 Uiso 1 1 calc R U . . . C34 C 0.24072(16) 0.69009(15) 0.57154(9) 0.0278(4) Uani 1 1 d . . . . . C42 C 0.29442(19) 0.98872(15) 0.77510(10) 0.0336(4) Uani 1 1 d . . . . . C68 C 0.38477(17) 0.41417(17) 0.91126(10) 0.0332(4) Uani 1 1 d . . . . . H68A H 0.376825 0.461543 0.886445 0.050 Uiso 1 1 calc R U . . . H68B H 0.383661 0.441880 0.956961 0.050 Uiso 1 1 calc R U . . . H68C H 0.327017 0.347155 0.893429 0.050 Uiso 1 1 calc R U . . . C32 C 0.54227(17) 0.99069(14) 0.57877(9) 0.0278(4) Uani 1 1 d . . . . . C12 C 0.66051(19) 0.88644(15) 0.80378(10) 0.0341(4) Uani 1 1 d . . . . . H12A H 0.606352 0.835208 0.817661 0.051 Uiso 1 1 calc R U . . . H12B H 0.669994 0.955578 0.828907 0.051 Uiso 1 1 calc R U . . . H12C H 0.726696 0.876265 0.811161 0.051 Uiso 1 1 calc R U . . . C8 C 0.59298(19) 0.57681(15) 0.61014(10) 0.0325(4) Uani 1 1 d . . . . . H8 H 0.586705 0.512264 0.583393 0.039 Uiso 1 1 calc R U . . . C30 C 0.54081(18) 0.82744(15) 0.52676(9) 0.0299(4) Uani 1 1 d . . . . . C45 C 0.17317(18) 0.84877(16) 0.66142(10) 0.0319(4) Uani 1 1 d . . . . . C11 C 0.70379(17) 0.96348(15) 0.71207(11) 0.0335(4) Uani 1 1 d . . . . . H11A H 0.775484 0.968184 0.725555 0.050 Uiso 1 1 calc R U . . . H11B H 0.697257 1.027812 0.733620 0.050 Uiso 1 1 calc R U . . . H11C H 0.687914 0.951611 0.664793 0.050 Uiso 1 1 calc R U . . . C14 C 0.3613(2) 0.44864(15) 0.54976(9) 0.0343(5) Uani 1 1 d . . . . . H14A H 0.351153 0.503272 0.532878 0.051 Uiso 1 1 calc R U . . . H14B H 0.293747 0.391407 0.542155 0.051 Uiso 1 1 calc R U . . . H14C H 0.409724 0.424409 0.527440 0.051 Uiso 1 1 calc R U . . . C47 C 0.75207(17) 0.48079(16) 0.90003(12) 0.0366(5) Uani 1 1 d . . . . . H47 H 0.753186 0.423603 0.914852 0.044 Uiso 1 1 calc R U . . . C51 C 0.89803(17) 0.92033(15) 0.92412(13) 0.0383(5) Uani 1 1 d . . . . . H51 H 0.893043 0.978501 0.952403 0.046 Uiso 1 1 calc R U . . . C7 C 0.68547(19) 0.66108(17) 0.62076(10) 0.0350(4) Uani 1 1 d . . . . . H7 H 0.741890 0.653716 0.601478 0.042 Uiso 1 1 calc R U . . . C48 C 0.82542(17) 0.57752(16) 0.92076(12) 0.0370(5) Uani 1 1 d . . . . . H48 H 0.887678 0.600958 0.952750 0.044 Uiso 1 1 calc R U . . . C15 C 0.4222(2) 0.40391(15) 0.64855(10) 0.0392(5) Uani 1 1 d . . . . . H15A H 0.473246 0.382343 0.627552 0.059 Uiso 1 1 calc R U . . . H15B H 0.355007 0.345459 0.638379 0.059 Uiso 1 1 calc R U . . . H15C H 0.447781 0.428379 0.695766 0.059 Uiso 1 1 calc R U . . . C39 C 0.21528(17) 0.72305(16) 0.51759(10) 0.0318(4) Uani 1 1 d . . . . . C31 C 0.57969(17) 0.93251(15) 0.53575(10) 0.0302(4) Uani 1 1 d . . . . . C53 C 0.97241(17) 0.85179(16) 0.83837(12) 0.0375(5) Uani 1 1 d . . . . . H53 H 1.017471 0.863129 0.808140 0.045 Uiso 1 1 calc R U . . . C43 C 0.1946(2) 0.98327(17) 0.75635(12) 0.0395(5) Uani 1 1 d . . . . . C55 C 0.77230(16) 0.80711(16) 0.97931(12) 0.0364(5) Uani 1 1 d . . . . . H55 H 0.706865 0.745098 0.958755 0.044 Uiso 1 1 calc R U . . . C26 C 0.3184(2) 0.87558(17) 0.90848(14) 0.0415(5) Uani 1 1 d . . . . . H26A H 0.262364 0.853730 0.870242 0.062 Uiso 1 1 calc R U . . . H26B H 0.365674 0.946565 0.913685 0.062 Uiso 1 1 calc R U . . . H26C H 0.287834 0.871545 0.947321 0.062 Uiso 1 1 calc R U . . . C35 C 0.19203(18) 0.58525(15) 0.56216(10) 0.0329(4) Uani 1 1 d . . . . . C52 C 0.96145(18) 0.93456(16) 0.87921(14) 0.0418(5) Uani 1 1 d . . . . . H52 H 0.998165 1.002074 0.876219 0.050 Uiso 1 1 calc R U . . . C44 C 0.13310(19) 0.91271(19) 0.69959(12) 0.0388(5) Uani 1 1 d . . . . . C69 C 0.5065(2) 0.33480(19) 0.94991(11) 0.0420(5) Uani 1 1 d . . . . . H69A H 0.453037 0.265030 0.933182 0.063 Uiso 1 1 calc R U . . . H69B H 0.501467 0.364459 0.994474 0.063 Uiso 1 1 calc R U . . . H69C H 0.576165 0.332305 0.949739 0.063 Uiso 1 1 calc R U . . . C38 C 0.15041(19) 0.6588(2) 0.45979(10) 0.0379(5) Uani 1 1 d . . . . . C56 C 0.74076(19) 0.8988(2) 1.00308(14) 0.0453(6) Uani 1 1 d . . . . . H56A H 0.802904 0.958650 1.027973 0.068 Uiso 1 1 calc R U . . . H56B H 0.689388 0.881688 1.030890 0.068 Uiso 1 1 calc R U . . . H56C H 0.709813 0.914682 0.965568 0.068 Uiso 1 1 calc R U . . . C70' C 0.7148(8) 0.3696(7) 0.7407(4) 0.0270(13) Uani 0.568(10) 1 d . . P A 2 H70' H 0.762963 0.429226 0.777341 0.032 Uiso 0.568(10) 1 calc R U P A 2 C57 C 0.8276(2) 0.7875(2) 1.03822(14) 0.0462(6) Uani 1 1 d . . . . . H57A H 0.837278 0.722363 1.024502 0.069 Uiso 1 1 calc R U . . . H57B H 0.784725 0.784128 1.071676 0.069 Uiso 1 1 calc R U . . . H57C H 0.896109 0.843693 1.055999 0.069 Uiso 1 1 calc R U . . . C37 C 0.10701(19) 0.5548(2) 0.45296(10) 0.0416(5) Uani 1 1 d . . . . . C23 C 0.2096(3) 0.3469(2) 0.74993(13) 0.0540(7) Uani 1 1 d . . . . . H23A H 0.283204 0.367735 0.770311 0.081 Uiso 1 1 calc R U . . . H23B H 0.196013 0.302716 0.705663 0.081 Uiso 1 1 calc R U . . . H23C H 0.164437 0.309122 0.775498 0.081 Uiso 1 1 calc R U . . . C24 C 0.0724(2) 0.4106(2) 0.71653(13) 0.0512(7) Uani 1 1 d . . . . . H24A H 0.027747 0.376206 0.743617 0.077 Uiso 1 1 calc R U . . . H24B H 0.057166 0.363357 0.673075 0.077 Uiso 1 1 calc R U . . . H24C H 0.058647 0.471722 0.712964 0.077 Uiso 1 1 calc R U . . . C36 C 0.1277(2) 0.51745(17) 0.50416(11) 0.0400(5) Uani 1 1 d . . . . . C100 C 1.0677(3) 0.9085(2) 0.36387(19) 0.0662(9) Uani 1 1 d . . . . . H10A H 1.032971 0.872762 0.318410 0.099 Uiso 1 1 calc R U . . . H10B H 1.122872 0.884181 0.376194 0.099 Uiso 1 1 calc R U . . . H10C H 1.098754 0.982690 0.368962 0.099 Uiso 1 1 calc R U . . . C72 C 0.7589(19) 0.3030(15) 0.7332(10) 0.058(5) Uani 0.432(10) 1 d . . P A 1 H72A H 0.777350 0.312389 0.780104 0.086 Uiso 0.432(10) 1 calc R U P A 1 H72B H 0.822916 0.320591 0.715317 0.086 Uiso 0.432(10) 1 calc R U P A 1 H72C H 0.713321 0.231192 0.711914 0.086 Uiso 0.432(10) 1 calc R U P A 1 B1 B 0.32697(17) 0.77570(15) 0.63583(9) 0.0236(4) Uani 1 1 d . . . . . C27 C 0.4694(2) 0.84043(18) 0.95767(13) 0.0478(6) Uani 1 1 d . . . . . H27A H 0.441346 0.840545 0.997628 0.072 Uiso 1 1 calc R U . . . H27B H 0.518194 0.909938 0.960664 0.072 Uiso 1 1 calc R U . . . H27C H 0.506401 0.793103 0.952067 0.072 Uiso 1 1 calc R U . . . C106 C 0.8871(3) 0.8923(2) 0.39229(16) 0.0587(7) Uani 1 1 d . . . . . H106 H 0.871966 0.910882 0.353692 0.070 Uiso 1 1 calc R U . . . C102 C 1.0030(3) 0.8587(3) 0.46615(17) 0.0614(8) Uani 1 1 d . . . . . H102 H 1.068550 0.853895 0.478826 0.074 Uiso 1 1 calc R U . . . C105 C 0.8133(2) 0.8719(2) 0.43089(16) 0.0560(7) Uani 1 1 d . . . . . H105 H 0.747848 0.876915 0.418616 0.067 Uiso 1 1 calc R U . . . C101 C 0.9835(3) 0.8856(2) 0.40977(18) 0.0622(8) Uani 1 1 d . . . . . C104 C 0.8332(3) 0.8440(2) 0.48741(16) 0.0598(7) Uani 1 1 d . . . . . H104 H 0.781518 0.829269 0.513346 0.072 Uiso 1 1 calc R U . . . C59 C 0.9553(8) 0.6772(5) 0.7378(4) 0.0408(16) Uani 0.432(10) 1 d . . P A 1 H59A H 0.903237 0.699139 0.717591 0.061 Uiso 0.432(10) 1 calc R U P A 1 H59B H 0.952360 0.612644 0.709273 0.061 Uiso 0.432(10) 1 calc R U P A 1 H59C H 1.025451 0.730205 0.744456 0.061 Uiso 0.432(10) 1 calc R U P A 1 C103 C 0.9273(3) 0.8382(3) 0.50509(18) 0.0683(9) Uani 1 1 d . . . . . H103 H 0.942154 0.820212 0.543979 0.082 Uiso 1 1 calc R U . . . C60 C 1.0172(5) 0.6350(5) 0.8376(3) 0.0418(18) Uani 0.432(10) 1 d . . P A 1 H60A H 1.084569 0.693511 0.850221 0.063 Uiso 0.432(10) 1 calc R U P A 1 H60B H 1.025749 0.574878 0.810899 0.063 Uiso 0.432(10) 1 calc R U P A 1 H60C H 0.993156 0.619452 0.876781 0.063 Uiso 0.432(10) 1 calc R U P A 1 C60' C 1.0509(4) 0.6775(4) 0.8098(3) 0.0505(17) Uani 0.568(10) 1 d . . P A 2 H60D H 1.092207 0.738914 0.797763 0.076 Uiso 0.568(10) 1 calc R U P A 2 H60E H 1.059698 0.617221 0.783478 0.076 Uiso 0.568(10) 1 calc R U P A 2 H60F H 1.075112 0.685886 0.855973 0.076 Uiso 0.568(10) 1 calc R U P A 2 C59' C 0.9036(6) 0.6531(5) 0.7204(3) 0.0426(12) Uani 0.568(10) 1 d . . P A 2 H59D H 0.828675 0.639125 0.708665 0.064 Uiso 0.568(10) 1 calc R U P A 2 H59E H 0.919087 0.596820 0.694619 0.064 Uiso 0.568(10) 1 calc R U P A 2 H59F H 0.944558 0.717712 0.711698 0.064 Uiso 0.568(10) 1 calc R U P A 2 C71' C 0.7127(6) 0.4037(5) 0.6784(4) 0.0412(14) Uani 0.568(10) 1 d . . P A 2 H71A H 0.664164 0.346436 0.642415 0.062 Uiso 0.568(10) 1 calc R U P A 2 H71B H 0.783197 0.425211 0.668557 0.062 Uiso 0.568(10) 1 calc R U P A 2 H71C H 0.689501 0.461543 0.684274 0.062 Uiso 0.568(10) 1 calc R U P A 2 C71 C 0.6831(6) 0.3724(6) 0.6514(4) 0.0313(14) Uani 0.432(10) 1 d . . P A 1 H71D H 0.640452 0.302320 0.624705 0.047 Uiso 0.432(10) 1 calc R U P A 1 H71E H 0.750463 0.396364 0.637691 0.047 Uiso 0.432(10) 1 calc R U P A 1 H71F H 0.646162 0.418035 0.645817 0.047 Uiso 0.432(10) 1 calc R U P A 1 C70 C 0.7014(10) 0.3732(10) 0.7212(4) 0.0267(19) Uani 0.432(10) 1 d . . P A 1 H70 H 0.747543 0.444936 0.746693 0.032 Uiso 0.432(10) 1 calc R U P A 1 C72' C 0.7573(13) 0.2838(8) 0.7325(8) 0.035(2) Uani 0.568(10) 1 d . . P A 2 H72D H 0.759057 0.261491 0.772374 0.052 Uiso 0.568(10) 1 calc R U P A 2 H72E H 0.828401 0.309287 0.723818 0.052 Uiso 0.568(10) 1 calc R U P A 2 H72F H 0.711844 0.225544 0.695915 0.052 Uiso 0.568(10) 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 As1 0.02296(9) 0.02776(9) 0.02041(9) 0.01251(7) 0.00767(6) 0.01226(7) Ga1 0.02141(10) 0.01830(9) 0.02929(11) 0.00348(8) 0.00367(7) 0.00597(7) Cl1 0.0290(2) 0.01929(19) 0.0455(3) 0.00579(18) 0.01199(19) 0.00457(16) P1 0.0218(2) 0.0222(2) 0.0251(2) 0.01100(17) 0.00945(16) 0.00917(16) Cl2 0.0219(2) 0.0367(3) 0.0447(3) -0.0004(2) 0.00054(19) 0.00566(18) Cl3 0.0414(3) 0.0433(3) 0.0464(3) 0.0242(2) 0.0131(2) 0.0228(2) Cl4 0.0415(3) 0.0424(3) 0.0381(3) -0.0049(2) 0.0074(2) 0.0206(2) F1 0.0553(8) 0.0176(5) 0.0247(5) 0.0070(4) 0.0119(5) 0.0153(5) F11 0.0441(7) 0.0264(5) 0.0245(5) 0.0020(4) 0.0015(5) 0.0145(5) F5 0.0500(7) 0.0184(5) 0.0311(6) 0.0058(4) 0.0153(5) 0.0142(5) F4 0.0517(8) 0.0175(5) 0.0355(6) 0.0086(5) 0.0132(5) 0.0080(5) F12 0.0708(10) 0.0247(6) 0.0304(6) 0.0058(5) 0.0178(6) 0.0180(6) F15 0.0371(7) 0.0466(7) 0.0388(7) 0.0135(6) 0.0024(5) 0.0183(6) F3 0.0541(8) 0.0323(6) 0.0418(7) 0.0176(6) 0.0251(6) 0.0151(6) F6 0.0546(8) 0.0209(5) 0.0324(6) 0.0077(5) -0.0074(6) 0.0065(5) F2 0.0662(9) 0.0316(6) 0.0354(7) 0.0114(5) 0.0272(6) 0.0251(6) F10 0.0419(7) 0.0373(6) 0.0323(6) 0.0209(5) 0.0018(5) 0.0120(5) F9 0.0496(8) 0.0692(10) 0.0225(6) 0.0185(6) -0.0010(5) 0.0221(7) N1 0.0255(7) 0.0140(6) 0.0143(6) 0.0038(5) 0.0034(5) 0.0039(5) N2 0.0213(7) 0.0163(6) 0.0169(6) 0.0057(5) 0.0026(5) 0.0060(5) F7 0.0626(10) 0.0250(6) 0.0486(8) -0.0051(6) -0.0118(7) 0.0052(6) F13 0.0734(11) 0.0409(8) 0.0626(9) 0.0210(7) 0.0397(8) 0.0355(8) F14 0.0465(8) 0.0597(9) 0.0653(10) 0.0299(8) 0.0222(7) 0.0335(7) F8 0.0591(9) 0.0603(10) 0.0261(7) -0.0075(6) -0.0117(6) 0.0133(8) N3 0.0213(7) 0.0168(6) 0.0363(8) 0.0089(6) 0.0023(6) 0.0059(5) N4 0.0208(7) 0.0183(7) 0.0380(9) 0.0075(6) 0.0014(6) 0.0076(6) C1 0.0222(7) 0.0146(7) 0.0152(7) 0.0050(6) 0.0026(6) 0.0053(6) C4 0.0294(8) 0.0188(7) 0.0148(7) 0.0056(6) 0.0067(6) 0.0079(6) C20 0.0247(8) 0.0268(8) 0.0199(8) 0.0048(7) 0.0055(6) 0.0101(7) C2 0.0294(8) 0.0143(7) 0.0161(7) 0.0032(6) 0.0006(6) 0.0065(6) C17 0.0188(7) 0.0197(7) 0.0236(8) 0.0053(6) 0.0049(6) 0.0064(6) C46 0.0196(8) 0.0168(7) 0.0288(8) 0.0064(6) 0.0050(6) 0.0065(6) C3 0.0257(8) 0.0188(7) 0.0187(7) 0.0050(6) 0.0004(6) 0.0082(6) C21 0.0195(7) 0.0206(7) 0.0205(7) 0.0057(6) 0.0032(6) 0.0080(6) C16 0.0180(7) 0.0208(7) 0.0186(7) 0.0079(6) 0.0048(6) 0.0082(6) C62 0.0260(8) 0.0182(7) 0.0268(8) 0.0108(7) 0.0055(7) 0.0085(6) C18 0.0226(8) 0.0227(8) 0.0295(9) 0.0080(7) 0.0090(7) 0.0041(6) C10 0.0300(9) 0.0163(7) 0.0248(8) 0.0053(6) 0.0046(7) 0.0042(6) C19 0.0240(8) 0.0305(9) 0.0255(8) 0.0103(7) 0.0107(7) 0.0087(7) C5 0.0309(9) 0.0188(7) 0.0195(7) 0.0080(6) 0.0080(6) 0.0066(7) C61 0.0228(8) 0.0144(7) 0.0333(9) 0.0078(7) 0.0043(7) 0.0057(6) C49 0.0181(8) 0.0172(7) 0.0409(10) 0.0062(7) 0.0004(7) 0.0051(6) C9 0.0413(10) 0.0186(8) 0.0168(7) 0.0061(6) 0.0093(7) 0.0088(7) C63 0.0252(8) 0.0187(8) 0.0337(9) 0.0111(7) 0.0089(7) 0.0062(6) C33 0.0378(10) 0.0198(8) 0.0195(8) 0.0045(6) 0.0044(7) 0.0118(7) C28 0.0364(10) 0.0193(8) 0.0156(7) 0.0055(6) 0.0019(6) 0.0107(7) C64 0.0291(9) 0.0154(7) 0.0361(10) 0.0065(7) 0.0078(7) 0.0044(7) C41 0.0448(11) 0.0226(8) 0.0253(9) 0.0105(7) 0.0111(8) 0.0151(8) C66 0.0296(9) 0.0158(8) 0.0486(12) 0.0078(8) 0.0182(8) 0.0066(7) C50 0.0201(8) 0.0215(8) 0.0458(11) 0.0044(8) 0.0038(8) 0.0069(7) C22 0.0249(8) 0.0209(8) 0.0237(8) 0.0028(7) 0.0042(7) 0.0038(7) C54 0.0203(8) 0.0207(8) 0.0410(10) 0.0049(7) 0.0026(7) 0.0069(7) C29 0.0430(11) 0.0180(8) 0.0202(8) 0.0075(6) 0.0051(7) 0.0129(7) C65 0.0367(10) 0.0153(7) 0.0395(11) 0.0035(7) 0.0166(8) 0.0067(7) C25 0.0291(9) 0.0189(7) 0.0203(8) 0.0042(6) 0.0036(6) 0.0055(7) C40 0.0390(10) 0.0232(8) 0.0225(8) 0.0114(7) 0.0071(7) 0.0142(7) C58 0.0245(9) 0.0240(9) 0.0444(11) 0.0002(8) 0.0030(8) 0.0075(7) C67 0.0344(10) 0.0257(8) 0.0239(8) 0.0112(7) 0.0063(7) 0.0084(7) C13 0.0461(11) 0.0158(7) 0.0189(8) 0.0024(6) 0.0066(7) 0.0053(7) C6 0.0352(10) 0.0284(9) 0.0303(9) 0.0133(8) 0.0151(8) 0.0086(8) C34 0.0350(10) 0.0268(9) 0.0198(8) 0.0067(7) 0.0006(7) 0.0107(8) C42 0.0555(13) 0.0226(9) 0.0292(9) 0.0118(8) 0.0177(9) 0.0168(9) C68 0.0392(11) 0.0345(10) 0.0279(9) 0.0121(8) 0.0150(8) 0.0116(9) C32 0.0405(10) 0.0176(8) 0.0238(8) 0.0070(7) 0.0047(7) 0.0089(7) C12 0.0515(13) 0.0213(8) 0.0237(9) 0.0045(7) 0.0063(8) 0.0084(8) C8 0.0535(13) 0.0252(9) 0.0237(9) 0.0076(7) 0.0199(8) 0.0167(9) C30 0.0478(12) 0.0255(9) 0.0222(8) 0.0081(7) 0.0122(8) 0.0185(8) C45 0.0417(11) 0.0311(9) 0.0307(10) 0.0165(8) 0.0104(8) 0.0173(8) C11 0.0374(11) 0.0209(8) 0.0343(10) 0.0103(8) 0.0039(8) 0.0010(8) C14 0.0597(14) 0.0205(8) 0.0184(8) 0.0026(7) 0.0030(8) 0.0132(9) C47 0.0297(10) 0.0235(9) 0.0547(13) 0.0143(9) -0.0054(9) 0.0099(8) C51 0.0325(10) 0.0189(8) 0.0603(14) 0.0040(9) 0.0097(10) 0.0100(8) C7 0.0469(12) 0.0352(10) 0.0314(10) 0.0140(8) 0.0237(9) 0.0182(9) C48 0.0275(10) 0.0261(9) 0.0550(13) 0.0143(9) -0.0072(9) 0.0100(8) C15 0.0644(15) 0.0182(8) 0.0222(9) 0.0054(7) -0.0003(9) 0.0029(9) C39 0.0365(10) 0.0347(10) 0.0236(9) 0.0107(8) 0.0029(7) 0.0119(8) C31 0.0416(11) 0.0258(9) 0.0258(9) 0.0118(7) 0.0108(8) 0.0120(8) C53 0.0296(10) 0.0256(9) 0.0530(13) 0.0098(9) 0.0118(9) 0.0049(8) C43 0.0602(15) 0.0307(10) 0.0444(12) 0.0206(9) 0.0304(11) 0.0252(10) C55 0.0236(9) 0.0283(9) 0.0505(13) 0.0026(9) 0.0093(8) 0.0061(7) C26 0.0459(13) 0.0272(10) 0.0585(14) 0.0164(10) 0.0152(11) 0.0179(9) C35 0.0436(11) 0.0260(9) 0.0228(9) 0.0035(7) -0.0038(8) 0.0107(8) C52 0.0355(11) 0.0191(9) 0.0661(16) 0.0106(10) 0.0129(11) 0.0045(8) C44 0.0444(12) 0.0419(12) 0.0479(13) 0.0272(10) 0.0209(10) 0.0252(10) C69 0.0565(14) 0.0398(12) 0.0329(11) 0.0205(9) 0.0053(10) 0.0167(11) C38 0.0427(12) 0.0514(13) 0.0197(9) 0.0113(9) 0.0011(8) 0.0185(10) C56 0.0340(11) 0.0429(13) 0.0551(15) -0.0010(11) 0.0111(10) 0.0179(10) C70' 0.030(3) 0.0188(18) 0.030(4) 0.004(3) 0.015(3) 0.0056(18) C57 0.0424(13) 0.0392(12) 0.0562(15) 0.0162(11) 0.0177(11) 0.0101(10) C37 0.0432(12) 0.0464(13) 0.0214(9) -0.0032(9) -0.0057(8) 0.0114(10) C23 0.081(2) 0.0448(14) 0.0370(12) -0.0072(11) -0.0076(12) 0.0422(14) C24 0.0396(13) 0.0642(17) 0.0371(12) -0.0109(12) -0.0124(10) 0.0253(12) C36 0.0460(13) 0.0282(10) 0.0325(11) -0.0019(8) -0.0038(9) 0.0076(9) C100 0.0575(18) 0.0468(15) 0.091(2) 0.0118(16) 0.0384(17) 0.0136(13) C72 0.043(7) 0.108(14) 0.045(7) 0.038(9) 0.021(5) 0.042(9) B1 0.0345(10) 0.0188(8) 0.0174(8) 0.0060(7) 0.0017(7) 0.0103(8) C27 0.0457(13) 0.0273(10) 0.0506(14) 0.0100(10) -0.0184(11) -0.0016(9) C106 0.073(2) 0.0339(12) 0.0614(17) 0.0086(12) 0.0100(15) 0.0141(13) C102 0.0538(17) 0.0612(18) 0.0641(19) 0.0032(15) 0.0030(14) 0.0266(14) C105 0.0493(15) 0.0457(14) 0.0618(17) 0.0054(13) 0.0004(13) 0.0133(12) C101 0.0634(18) 0.0338(13) 0.075(2) -0.0007(13) 0.0189(16) 0.0084(12) C104 0.0545(17) 0.0515(16) 0.0621(18) 0.0071(14) 0.0065(14) 0.0132(13) C59 0.047(4) 0.038(3) 0.036(3) 0.004(3) 0.016(3) 0.015(3) C103 0.071(2) 0.067(2) 0.0619(19) 0.0094(16) -0.0005(16) 0.0290(17) C60 0.042(3) 0.042(3) 0.046(3) 0.001(3) 0.008(2) 0.028(3) C60' 0.034(2) 0.047(3) 0.066(4) -0.002(3) 0.002(2) 0.022(2) C59' 0.044(3) 0.051(3) 0.031(2) 0.002(2) 0.010(2) 0.021(3) C71' 0.045(3) 0.035(3) 0.059(4) 0.024(3) 0.032(3) 0.021(2) C71 0.032(3) 0.035(3) 0.032(3) 0.015(3) 0.014(2) 0.014(3) C70 0.028(3) 0.023(3) 0.023(4) 0.003(3) 0.011(3) 0.004(2) C72' 0.028(3) 0.030(2) 0.046(5) 0.003(2) 0.007(3) 0.0156(19) 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 As1 P1 103.95(5) Cl4 Ga1 Cl1 108.18(2) Cl4 Ga1 Cl3 111.60(2) Cl1 Ga1 Cl3 106.53(2) Cl4 Ga1 Cl2 112.79(2) Cl1 Ga1 Cl2 107.99(2) Cl3 Ga1 Cl2 109.49(2) C46 P1 As1 93.30(6) C1 N1 C2 110.58(14) C1 N1 C4 119.03(14) C2 N1 C4 129.81(14) C1 N2 C3 109.43(14) C1 N2 C16 126.21(14) C3 N2 C16 124.35(14) C46 N3 C47 109.17(15) C46 N3 C61 125.80(15) C47 N3 C61 124.56(15) C46 N4 C48 109.62(16) C46 N4 C49 122.95(16) C48 N4 C49 126.76(16) N2 C1 N1 106.33(14) N2 C1 As1 117.09(11) N1 C1 As1 136.34(13) C5 C4 C9 123.71(17) C5 C4 N1 118.99(15) C9 C4 N1 117.17(15) C19 C20 C21 120.61(16) C3 C2 N1 103.99(14) C3 C2 B1 119.88(16) N1 C2 B1 136.08(16) C18 C17 C16 116.03(16) C18 C17 C22 120.84(16) C16 C17 C22 123.10(15) N4 C46 N3 106.82(15) N4 C46 P1 122.04(13) N3 C46 P1 130.05(14) N2 C3 C2 109.65(16) C20 C21 C16 116.37(16) C20 C21 C25 120.64(15) C16 C21 C25 122.96(15) C17 C16 C21 124.82(15) C17 C16 N2 117.75(14) C21 C16 N2 117.35(14) C63 C62 C61 116.56(17) C63 C62 C67 120.77(17) C61 C62 C67 122.37(17) C19 C18 C17 121.14(17) C5 C10 C11 112.44(16) C5 C10 C12 112.18(15) C11 C10 C12 109.17(16) C18 C19 C20 121.01(17) C6 C5 C4 116.29(16) C6 C5 C10 121.62(17) C4 C5 C10 122.08(16) C66 C61 C62 123.97(17) C66 C61 N3 117.54(16) C62 C61 N3 118.44(17) C54 C49 C50 123.84(17) C54 C49 N4 116.88(17) C50 C49 N4 119.28(18) C8 C9 C4 116.86(18) C8 C9 C13 119.84(17) C4 C9 C13 123.27(18) C64 C63 C62 121.16(17) F5 C33 C32 114.46(16) F5 C33 C28 121.03(17) C32 C33 C28 124.47(17) C29 C28 C33 112.36(17) C29 C28 B1 119.62(16) C33 C28 B1 127.29(17) C65 C64 C63 120.58(18) F11 C41 C42 115.59(19) F11 C41 C40 119.68(17) C42 C41 C40 124.7(2) C65 C66 C61 116.73(17) C65 C66 C70' 123.7(4) C61 C66 C70' 118.9(4) C65 C66 C70 114.6(4) C61 C66 C70 128.3(5) C51 C50 C49 116.2(2) C51 C50 C55 121.17(19) C49 C50 C55 122.64(18) C24 C22 C17 111.49(17) C24 C22 C23 109.7(2) C17 C22 C23 111.79(16) C53 C54 C49 117.11(18) C53 C54 C58 119.88(19) C49 C54 C58 122.99(18) F1 C29 C30 114.98(16) F1 C29 C28 119.80(17) C30 C29 C28 125.17(17) C64 C65 C66 120.87(19) C26 C25 C21 111.36(16) C26 C25 C27 110.32(19) C21 C25 C27 111.62(16) C45 C40 C41 113.01(18) C45 C40 B1 127.11(17) C41 C40 B1 119.76(17) C59 C58 C54 113.7(3) C54 C58 C60' 110.1(2) C59 C58 C60 114.7(4) C54 C58 C60 108.4(3) C54 C58 C59' 112.8(2) C60' C58 C59' 105.3(3) C62 C67 C68 113.89(16) C62 C67 C69 108.62(17) C68 C67 C69 109.97(18) C9 C13 C15 112.22(18) C9 C13 C14 111.19(16) C15 C13 C14 108.37(15) C7 C6 C5 121.44(19) C35 C34 C39 113.45(17) C35 C34 B1 127.79(16) C39 C34 B1 118.68(17) F12 C42 C43 119.96(19) F12 C42 C41 120.7(2) C43 C42 C41 119.3(2) F4 C32 C31 119.51(18) F4 C32 C33 120.23(17) C31 C32 C33 120.25(17) C7 C8 C9 121.29(18) F2 C30 C29 120.68(17) F2 C30 C31 119.82(18) C29 C30 C31 119.49(18) F15 C45 C40 121.79(18) F15 C45 C44 114.3(2) C40 C45 C44 123.9(2) C48 C47 N3 107.37(17) C52 C51 C50 121.4(2) C8 C7 C6 120.41(19) C47 C48 N4 107.02(18) F10 C39 C38 116.05(18) F10 C39 C34 119.52(17) C38 C39 C34 124.4(2) F3 C31 C32 120.92(17) F3 C31 C30 120.83(18) C32 C31 C30 118.24(18) C52 C53 C54 120.7(2) F13 C43 C42 120.4(2) F13 C43 C44 120.4(2) C42 C43 C44 119.2(2) C50 C55 C56 112.6(2) C50 C55 C57 110.91(18) C56 C55 C57 109.0(2) F6 C35 C34 121.12(17) F6 C35 C36 114.92(18) C34 C35 C36 123.96(19) C51 C52 C53 120.8(2) F14 C44 C43 120.3(2) F14 C44 C45 119.8(2) C43 C44 C45 119.9(2) F9 C38 C39 120.8(2) F9 C38 C37 119.98(19) C39 C38 C37 119.2(2) C66 C70' C71' 107.7(5) C66 C70' C72' 113.9(8) C71' C70' C72' 109.0(9) F8 C37 C36 120.2(2) F8 C37 C38 120.3(2) C36 C37 C38 119.43(19) F7 C36 C37 120.4(2) F7 C36 C35 120.1(2) C37 C36 C35 119.5(2) C28 B1 C34 104.78(14) C28 B1 C2 115.39(15) C34 B1 C2 111.42(14) C28 B1 C40 112.97(14) C34 B1 C40 110.79(16) C2 B1 C40 101.67(14) C105 C106 C101 120.1(3) C101 C102 C103 120.8(3) C106 C105 C104 121.1(3) C102 C101 C106 118.5(3) C102 C101 C100 122.1(3) C106 C101 C100 119.3(3) C103 C104 C105 119.1(3) C104 C103 C102 120.3(3) C71 C70 C72 112.1(12) C71 C70 C66 119.1(8) C72 C70 C66 103.0(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance As1 C1 1.9444(16) As1 P1 2.1577(5) Ga1 Cl4 2.1639(6) Ga1 Cl1 2.1719(5) Ga1 Cl3 2.1767(6) Ga1 Cl2 2.1791(5) P1 C46 1.8445(18) F1 C29 1.352(2) F11 C41 1.341(3) F5 C33 1.351(2) F4 C32 1.348(2) F12 C42 1.341(3) F15 C45 1.350(3) F3 C31 1.336(2) F6 C35 1.352(2) F2 C30 1.341(2) F10 C39 1.348(2) F9 C38 1.341(2) N1 C1 1.367(2) N1 C2 1.398(2) N1 C4 1.451(2) N2 C1 1.345(2) N2 C3 1.363(2) N2 C16 1.452(2) F7 C36 1.343(3) F13 C43 1.344(2) F14 C44 1.342(3) F8 C37 1.345(2) N3 C46 1.352(2) N3 C47 1.379(3) N3 C61 1.451(2) N4 C46 1.347(2) N4 C48 1.377(2) N4 C49 1.451(2) C4 C5 1.406(2) C4 C9 1.407(2) C20 C19 1.388(3) C20 C21 1.398(2) C2 C3 1.373(3) C2 B1 1.665(2) C17 C18 1.396(2) C17 C16 1.399(2) C17 C22 1.520(2) C21 C16 1.399(2) C21 C25 1.519(2) C62 C63 1.392(3) C62 C61 1.399(3) C62 C67 1.523(3) C18 C19 1.385(3) C10 C5 1.524(2) C10 C11 1.529(3) C10 C12 1.533(3) C5 C6 1.396(3) C61 C66 1.398(3) C49 C54 1.393(3) C49 C50 1.404(3) C9 C8 1.387(3) C9 C13 1.526(3) C63 C64 1.386(3) C33 C32 1.380(3) C33 C28 1.395(2) C28 C29 1.393(3) C28 B1 1.654(3) C64 C65 1.384(3) C41 C42 1.386(3) C41 C40 1.401(3) C66 C65 1.396(3) C66 C70' 1.518(10) C66 C70 1.570(13) C50 C51 1.396(3) C50 C55 1.516(3) C22 C24 1.513(3) C22 C23 1.524(3) C54 C53 1.392(3) C54 C58 1.519(3) C29 C30 1.380(3) C25 C26 1.518(3) C25 C27 1.527(3) C40 C45 1.388(3) C40 B1 1.668(3) C58 C59 1.390(7) C58 C60' 1.545(5) C58 C60 1.576(6) C58 C59' 1.627(6) C67 C68 1.524(3) C67 C69 1.537(3) C13 C15 1.534(3) C13 C14 1.542(3) C6 C7 1.387(3) C34 C35 1.383(3) C34 C39 1.401(3) C34 B1 1.657(3) C42 C43 1.370(4) C32 C31 1.375(3) C8 C7 1.384(3) C30 C31 1.381(3) C45 C44 1.396(3) C47 C48 1.353(3) C51 C52 1.375(4) C39 C38 1.376(3) C53 C52 1.382(3) C43 C44 1.374(4) C55 C56 1.532(3) C55 C57 1.539(4) C35 C36 1.391(3) C38 C37 1.376(4) C70' C71' 1.525(8) C70' C72' 1.527(16) C37 C36 1.371(3) C100 C101 1.603(5) C72 C70 1.53(2) C106 C105 1.379(5) C106 C101 1.391(5) C102 C101 1.378(5) C102 C103 1.404(5) C105 C104 1.389(5) C104 C103 1.356(5) C71 C70 1.493(10) 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 C3 N2 C1 N1 -1.23(18) C16 N2 C1 N1 -179.90(14) C3 N2 C1 As1 174.09(11) C16 N2 C1 As1 -4.6(2) C2 N1 C1 N2 1.04(18) C4 N1 C1 N2 -171.06(14) C2 N1 C1 As1 -172.92(13) C4 N1 C1 As1 15.0(2) C1 N1 C4 C5 -102.48(18) C2 N1 C4 C5 87.2(2) C1 N1 C4 C9 73.4(2) C2 N1 C4 C9 -96.9(2) C1 N1 C2 C3 -0.44(18) C4 N1 C2 C3 170.56(16) C1 N1 C2 B1 177.17(17) C4 N1 C2 B1 -11.8(3) C48 N4 C46 N3 0.2(2) C49 N4 C46 N3 171.37(17) C48 N4 C46 P1 -168.98(15) C49 N4 C46 P1 2.2(3) C47 N3 C46 N4 -0.1(2) C61 N3 C46 N4 -172.46(17) C47 N3 C46 P1 167.89(16) C61 N3 C46 P1 -4.5(3) As1 P1 C46 N4 -119.57(15) As1 P1 C46 N3 74.02(17) C1 N2 C3 C2 1.00(19) C16 N2 C3 C2 179.69(15) N1 C2 C3 N2 -0.33(18) B1 C2 C3 N2 -178.42(14) C19 C20 C21 C16 -0.8(3) C19 C20 C21 C25 177.25(17) C18 C17 C16 C21 -2.0(3) C22 C17 C16 C21 176.04(16) C18 C17 C16 N2 -178.63(15) C22 C17 C16 N2 -0.6(2) C20 C21 C16 C17 2.1(3) C25 C21 C16 C17 -175.92(16) C20 C21 C16 N2 178.77(15) C25 C21 C16 N2 0.8(2) C1 N2 C16 C17 -90.7(2) C3 N2 C16 C17 90.9(2) C1 N2 C16 C21 92.4(2) C3 N2 C16 C21 -86.1(2) C16 C17 C18 C19 0.6(3) C22 C17 C18 C19 -177.48(17) C17 C18 C19 C20 0.6(3) C21 C20 C19 C18 -0.5(3) C9 C4 C5 C6 0.4(3) N1 C4 C5 C6 176.04(16) C9 C4 C5 C10 179.58(17) N1 C4 C5 C10 -4.8(2) C11 C10 C5 C6 27.4(3) C12 C10 C5 C6 -96.1(2) C11 C10 C5 C4 -151.73(17) C12 C10 C5 C4 84.8(2) C63 C62 C61 C66 -3.6(3) C67 C62 C61 C66 170.15(18) C63 C62 C61 N3 179.01(15) C67 C62 C61 N3 -7.2(2) C46 N3 C61 C66 81.7(2) C47 N3 C61 C66 -89.5(3) C46 N3 C61 C62 -100.7(2) C47 N3 C61 C62 88.0(2) C46 N4 C49 C54 -83.2(2) C48 N4 C49 C54 86.4(3) C46 N4 C49 C50 95.9(2) C48 N4 C49 C50 -94.5(3) C5 C4 C9 C8 -0.2(3) N1 C4 C9 C8 -175.91(16) C5 C4 C9 C13 -178.23(17) N1 C4 C9 C13 6.1(3) C61 C62 C63 C64 0.6(3) C67 C62 C63 C64 -173.28(17) F5 C33 C28 C29 176.35(16) C32 C33 C28 C29 -1.2(3) F5 C33 C28 B1 6.3(3) C32 C33 C28 B1 -171.27(18) C62 C63 C64 C65 2.1(3) C62 C61 C66 C65 3.7(3) N3 C61 C66 C65 -178.87(17) C62 C61 C66 C70' -166.8(4) N3 C61 C66 C70' 10.6(4) C62 C61 C66 C70 176.0(5) N3 C61 C66 C70 -6.5(6) C54 C49 C50 C51 1.1(3) N4 C49 C50 C51 -177.84(18) C54 C49 C50 C55 -177.47(19) N4 C49 C50 C55 3.6(3) C18 C17 C22 C24 64.2(3) C16 C17 C22 C24 -113.7(2) C18 C17 C22 C23 -59.0(3) C16 C17 C22 C23 123.1(2) C50 C49 C54 C53 -1.6(3) N4 C49 C54 C53 177.42(18) C50 C49 C54 C58 176.74(19) N4 C49 C54 C58 -4.3(3) C33 C28 C29 F1 -176.75(16) B1 C28 C29 F1 -5.8(3) C33 C28 C29 C30 0.5(3) B1 C28 C29 C30 171.44(18) C63 C64 C65 C66 -2.0(3) C61 C66 C65 C64 -0.8(3) C70' C66 C65 C64 169.2(4) C70 C66 C65 C64 -174.2(5) C20 C21 C25 C26 -66.7(2) C16 C21 C25 C26 111.2(2) C20 C21 C25 C27 57.0(2) C16 C21 C25 C27 -125.0(2) F11 C41 C40 C45 178.85(16) C42 C41 C40 C45 -1.5(3) F11 C41 C40 B1 2.6(3) C42 C41 C40 B1 -177.79(17) C53 C54 C58 C59 -32.1(5) C49 C54 C58 C59 149.7(5) C53 C54 C58 C60' 57.6(4) C49 C54 C58 C60' -120.6(4) C53 C54 C58 C60 96.7(4) C49 C54 C58 C60 -81.5(4) C53 C54 C58 C59' -59.6(4) C49 C54 C58 C59' 122.1(3) C63 C62 C67 C68 -46.8(2) C61 C62 C67 C68 139.73(18) C63 C62 C67 C69 76.1(2) C61 C62 C67 C69 -97.4(2) C8 C9 C13 C15 63.3(2) C4 C9 C13 C15 -118.7(2) C8 C9 C13 C14 -58.3(2) C4 C9 C13 C14 119.7(2) C4 C5 C6 C7 -0.6(3) C10 C5 C6 C7 -179.73(18) F11 C41 C42 F12 0.0(3) C40 C41 C42 F12 -179.64(17) F11 C41 C42 C43 179.97(17) C40 C41 C42 C43 0.3(3) F5 C33 C32 F4 2.1(3) C28 C33 C32 F4 179.79(17) F5 C33 C32 C31 -176.74(18) C28 C33 C32 C31 0.9(3) C4 C9 C8 C7 0.1(3) C13 C9 C8 C7 178.24(19) F1 C29 C30 F2 -1.2(3) C28 C29 C30 F2 -178.54(18) F1 C29 C30 C31 177.79(18) C28 C29 C30 C31 0.4(3) C41 C40 C45 F15 -177.26(17) B1 C40 C45 F15 -1.3(3) C41 C40 C45 C44 1.5(3) B1 C40 C45 C44 177.51(18) C46 N3 C47 C48 0.0(3) C61 N3 C47 C48 172.4(2) C49 C50 C51 C52 0.5(3) C55 C50 C51 C52 179.1(2) C9 C8 C7 C6 -0.3(3) C5 C6 C7 C8 0.5(3) N3 C47 C48 N4 0.2(3) C46 N4 C48 C47 -0.2(3) C49 N4 C48 C47 -171.0(2) C35 C34 C39 F10 176.11(19) B1 C34 C39 F10 -6.9(3) C35 C34 C39 C38 -1.5(3) B1 C34 C39 C38 175.5(2) F4 C32 C31 F3 0.2(3) C33 C32 C31 F3 179.07(19) F4 C32 C31 C30 -178.77(18) C33 C32 C31 C30 0.1(3) F2 C30 C31 F3 -0.7(3) C29 C30 C31 F3 -179.70(19) F2 C30 C31 C32 178.24(19) C29 C30 C31 C32 -0.7(3) C49 C54 C53 C52 0.4(3) C58 C54 C53 C52 -177.9(2) F12 C42 C43 F13 0.4(3) C41 C42 C43 F13 -179.55(18) F12 C42 C43 C44 -179.09(18) C41 C42 C43 C44 1.0(3) C51 C50 C55 C56 21.8(3) C49 C50 C55 C56 -159.7(2) C51 C50 C55 C57 -100.7(2) C49 C50 C55 C57 77.8(3) C39 C34 C35 F6 -177.1(2) B1 C34 C35 F6 6.3(4) C39 C34 C35 C36 2.8(3) B1 C34 C35 C36 -173.9(2) C50 C51 C52 C53 -1.5(4) C54 C53 C52 C51 1.1(4) F13 C43 C44 F14 -1.4(3) C42 C43 C44 F14 178.12(19) F13 C43 C44 C45 179.61(19) C42 C43 C44 C45 -0.9(3) F15 C45 C44 F14 -0.6(3) C40 C45 C44 F14 -179.46(18) F15 C45 C44 C43 178.46(19) C40 C45 C44 C43 -0.4(3) F10 C39 C38 F9 1.5(3) C34 C39 C38 F9 179.2(2) F10 C39 C38 C37 -178.1(2) C34 C39 C38 C37 -0.4(4) C65 C66 C70' C71' 68.8(7) C61 C66 C70' C71' -121.4(5) C65 C66 C70' C72' -52.2(9) C61 C66 C70' C72' 117.6(8) F9 C38 C37 F8 -1.0(4) C39 C38 C37 F8 178.7(2) F9 C38 C37 C36 -178.4(2) C39 C38 C37 C36 1.2(4) F8 C37 C36 F7 2.7(4) C38 C37 C36 F7 -179.8(2) F8 C37 C36 C35 -177.4(2) C38 C37 C36 C35 0.1(4) F6 C35 C36 F7 -2.5(4) C34 C35 C36 F7 177.7(2) F6 C35 C36 C37 177.6(2) C34 C35 C36 C37 -2.2(4) C29 C28 B1 C34 -48.5(2) C33 C28 B1 C34 120.99(19) C29 C28 B1 C2 74.5(2) C33 C28 B1 C2 -116.09(19) C29 C28 B1 C40 -169.15(16) C33 C28 B1 C40 0.3(3) C35 C34 B1 C28 128.2(2) C39 C34 B1 C28 -48.3(2) C35 C34 B1 C2 2.7(3) C39 C34 B1 C2 -173.76(18) C35 C34 B1 C40 -109.7(2) C39 C34 B1 C40 73.8(2) C3 C2 B1 C28 158.04(16) N1 C2 B1 C28 -19.3(3) C3 C2 B1 C34 -82.6(2) N1 C2 B1 C34 100.0(2) C3 C2 B1 C40 35.4(2) N1 C2 B1 C40 -141.92(19) C45 C40 B1 C28 116.3(2) C41 C40 B1 C28 -68.0(2) C45 C40 B1 C34 -0.9(3) C41 C40 B1 C34 174.81(16) C45 C40 B1 C2 -119.43(19) C41 C40 B1 C2 56.3(2) C101 C106 C105 C104 -0.3(4) C103 C102 C101 C106 0.1(5) C103 C102 C101 C100 -179.5(3) C105 C106 C101 C102 -0.2(4) C105 C106 C101 C100 179.4(3) C106 C105 C104 C103 0.8(5) C105 C104 C103 C102 -0.9(5) C101 C102 C103 C104 0.4(5) C65 C66 C70 C71 42.3(11) C61 C66 C70 C71 -130.2(7) C65 C66 C70 C72 -82.5(10) C61 C66 C70 C72 105.0(10)