#------------------------------------------------------------------------------ #$Date: 2014-12-22 15:48:03 +0200 (Mon, 22 Dec 2014) $ #$Revision: 128995 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116061.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_7116061 loop_ _publ_author_name 'Laura H. Davies' 'Benjamin B. Kasten' 'Paul D. Benny' 'Rory L. Arrowsmith' 'Haobo Ge'Sofia I. Pascu' 'Stan W. Botchway' 'William Clegg' 'Ross W. Harrington' 'Lee J. Higham' _publ_section_title ; Re and ^99m^Tc complexes of BodP3 - multi-modality imaging probes ; _journal_name_full Chem.Commun. _journal_page_first 15503 _journal_paper_doi 10.1039/C4cc06367H _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C55 H60 B Cl N2 O2 P3 Re' _chemical_formula_sum 'C55 H60 B Cl N2 O2 P3 Re' _chemical_formula_weight 1106.42 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 106.521(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.7603(4) _cell_length_b 26.1035(8) _cell_length_c 15.6208(4) _cell_measurement_reflns_used 6037 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 62.34 _cell_measurement_theta_min 2.95 _cell_volume 4988.3(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.3968 _diffrn_measured_fraction_theta_full 0.855 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device_type 'Agilent Technologies Gemini A Ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_laue_measured_fraction_full 0.855 _diffrn_reflns_laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16817 _diffrn_reflns_point_group_measured_fraction_full 0.855 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 62.424 _diffrn_reflns_theta_min 3.386 _diffrn_source 'sealed tube with Enhance Ultra optics' _exptl_absorpt_coefficient_mu 6.500 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_correction_T_min 0.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2248 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.240 _refine_diff_density_min -1.306 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 594 _refine_ls_number_reflns 7730 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0408 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.1001 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6049 _reflns_number_total 7730 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc06367h2.cif _[local]_cod_data_source_block ljh117 _cod_database_code 7116061 _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 0.442 _shelx_estimated_absorpt_t_max 0.881 _shelxl_version_number 2014-3 _shelx_res_file ; TITL ljh117 in P2(1)/c CELL 1.54178 12.7603 26.1035 15.6208 90.000 106.521 90.000 ZERR 4.00 0.0004 0.0008 0.0004 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O N P CL RE B UNIT 220 240 8 8 12 4 4 4 REM red plate SIZE 0.15 0.10 0.02 TEMP -123 L.S. 8 ACTA BOND $H CONF FMAP 2 PLAN 10 REM EXTI 0.000000 WGHT 0.045700 FVAR 0.52301 RE 7 0.210673 0.172753 0.479184 11.00000 0.02648 0.02370 = 0.01895 -0.00037 0.00415 0.00130 B 8 0.287101 0.578463 0.523305 11.00000 0.04133 0.02986 = 0.03827 -0.00442 0.01047 -0.00822 N1 4 0.377887 0.544439 0.592014 11.00000 0.04257 0.03238 = 0.03442 -0.00757 0.01099 -0.00650 N2 4 0.193305 0.539351 0.476136 11.00000 0.04171 0.02574 = 0.03629 -0.00348 0.01159 0.00059 C1 1 0.475785 0.560662 0.643393 11.00000 0.04495 0.04319 = 0.04003 -0.01413 0.01420 -0.00602 C2 1 0.535265 0.518746 0.691086 11.00000 0.04156 0.05891 = 0.03024 -0.01176 0.01303 -0.00822 C3 1 0.470573 0.475394 0.669478 11.00000 0.04421 0.04593 = 0.02931 -0.00387 0.00978 0.00254 C4 1 0.371154 0.491893 0.605909 11.00000 0.03685 0.03377 = 0.02738 -0.00640 0.00688 -0.00323 C5 1 0.279444 0.463603 0.558232 11.00000 0.04794 0.02956 = 0.02420 -0.00580 0.01324 -0.00300 C6 1 0.194858 0.486454 0.493842 11.00000 0.03222 0.01541 = 0.02649 0.00343 0.00058 -0.00543 C7 1 0.095313 0.464627 0.438003 11.00000 0.04087 0.02873 = 0.03077 0.00015 0.01249 0.00032 C8 1 0.039931 0.503937 0.385318 11.00000 0.04238 0.03508 = 0.03555 0.00105 0.01197 0.00015 C9 1 0.101296 0.549371 0.409609 11.00000 0.04357 0.03482 = 0.03416 0.00141 0.01252 0.00152 C10 1 0.514117 0.613764 0.651334 11.00000 0.04973 0.05965 = 0.05573 -0.02128 0.01456 -0.01784 AFIX 137 H10A 2 0.478489 0.632320 0.596198 11.00000 -1.50000 H10B 2 0.593497 0.614336 0.661387 11.00000 -1.50000 H10C 2 0.496035 0.630197 0.701735 11.00000 -1.50000 AFIX 0 C11 1 0.647485 0.521785 0.754032 11.00000 0.04077 0.07736 = 0.03667 -0.00971 0.00789 -0.01221 AFIX 23 H11A 2 0.657901 0.492803 0.796508 11.00000 -1.20000 H11B 2 0.653948 0.553880 0.788916 11.00000 -1.20000 AFIX 0 C12 1 0.738078 0.520459 0.708280 11.00000 0.05011 0.10270 = 0.04833 -0.02877 0.01448 -0.00030 AFIX 137 H12A 2 0.808689 0.526444 0.752572 11.00000 -1.50000 H12B 2 0.725050 0.547201 0.662419 11.00000 -1.50000 H12C 2 0.738805 0.486879 0.680400 11.00000 -1.50000 AFIX 0 C13 1 0.498727 0.423344 0.708471 11.00000 0.04127 0.06475 = 0.03458 -0.00143 0.00326 0.00659 AFIX 137 H13A 2 0.576122 0.422408 0.742563 11.00000 -1.50000 H13B 2 0.484939 0.397947 0.660345 11.00000 -1.50000 H13C 2 0.453631 0.415455 0.748144 11.00000 -1.50000 AFIX 0 C14 1 0.055907 0.410498 0.431017 11.00000 0.03831 0.04181 = 0.04094 0.00160 -0.00300 -0.01499 AFIX 137 H14A 2 -0.022307 0.409585 0.399372 11.00000 -1.50000 H14B 2 0.067945 0.396168 0.491029 11.00000 -1.50000 H14C 2 0.096222 0.390219 0.398066 11.00000 -1.50000 AFIX 0 C15 1 -0.065461 0.499756 0.311559 11.00000 0.03429 0.05199 = 0.04110 0.00254 0.00381 0.00076 AFIX 23 H15A 2 -0.099249 0.534147 0.300017 11.00000 -1.20000 H15B 2 -0.116274 0.477343 0.331853 11.00000 -1.20000 AFIX 0 C16 1 -0.052034 0.478687 0.225217 11.00000 0.04315 0.06655 = 0.04229 -0.00210 0.00226 -0.00499 AFIX 137 H16A 2 -0.123310 0.477821 0.180061 11.00000 -1.50000 H16B 2 -0.022075 0.443915 0.235195 11.00000 -1.50000 H16C 2 -0.002007 0.500657 0.204387 11.00000 -1.50000 AFIX 0 C17 1 0.071837 0.600772 0.368617 11.00000 0.05901 0.04053 = 0.05809 0.01278 0.01112 0.00845 AFIX 137 H17A 2 0.125356 0.626086 0.400791 11.00000 -1.50000 H17B 2 -0.001072 0.610347 0.372163 11.00000 -1.50000 H17C 2 0.071827 0.599731 0.305902 11.00000 -1.50000 AFIX 0 C18 1 0.342370 0.601587 0.449881 11.00000 0.05879 0.03754 = 0.05439 0.00262 0.02162 -0.00595 AFIX 137 H18A 2 0.385029 0.574778 0.431282 11.00000 -1.50000 H18B 2 0.390541 0.630184 0.476205 11.00000 -1.50000 H18C 2 0.284892 0.613754 0.397848 11.00000 -1.50000 AFIX 0 C19 1 0.238927 0.618780 0.580297 11.00000 0.04817 0.03942 = 0.05315 -0.00620 0.01979 -0.00542 AFIX 137 H19A 2 0.207727 0.600208 0.621790 11.00000 -1.50000 H19B 2 0.181891 0.639474 0.539756 11.00000 -1.50000 H19C 2 0.297825 0.641213 0.614054 11.00000 -1.50000 AFIX 0 C20 1 0.274292 0.408099 0.573071 11.00000 0.03431 0.03003 = 0.02718 0.00138 0.00254 0.00409 C21 1 0.300905 0.373439 0.515116 11.00000 0.04733 0.03149 = 0.03161 0.00057 0.01647 -0.00213 AFIX 43 H21 2 0.330706 0.385785 0.469805 11.00000 -1.20000 AFIX 0 C22 1 0.285106 0.321656 0.521819 11.00000 0.04663 0.03156 = 0.02561 -0.00795 0.01468 -0.00184 AFIX 43 H22 2 0.303552 0.298779 0.481066 11.00000 -1.20000 AFIX 0 C23 1 0.241962 0.302454 0.588405 11.00000 0.03009 0.03231 = 0.02013 0.00328 0.00379 0.00399 C24 1 0.223586 0.337002 0.650850 11.00000 0.04121 0.03783 = 0.02283 0.00017 0.01049 0.00908 AFIX 43 H24 2 0.199767 0.324537 0.699325 11.00000 -1.20000 AFIX 0 C25 1 0.239434 0.389043 0.643407 11.00000 0.05101 0.02253 = 0.02757 -0.00357 0.01251 0.00676 AFIX 43 H25 2 0.226414 0.411881 0.686623 11.00000 -1.20000 AFIX 0 P1 5 0.405117 0.174735 0.545075 11.00000 0.02820 0.02245 = 0.02142 -0.00269 0.00262 0.00078 P2 5 0.221119 0.234236 0.596902 11.00000 0.02990 0.02355 = 0.01894 -0.00051 0.00484 0.00323 P3 5 0.017670 0.189278 0.451301 11.00000 0.02712 0.02950 = 0.02400 0.00044 0.00398 0.00389 C26 1 0.491004 0.201615 0.479640 11.00000 0.02732 0.02902 = 0.02732 0.00464 0.00497 -0.00025 C27 1 0.565744 0.240927 0.508079 11.00000 0.04053 0.04577 = 0.03547 -0.00601 0.00833 -0.00512 AFIX 43 H27 2 0.573258 0.256553 0.564433 11.00000 -1.20000 AFIX 0 C28 1 0.629531 0.257690 0.455417 11.00000 0.04354 0.03857 = 0.04622 -0.00006 0.01866 -0.01384 AFIX 43 H28 2 0.681080 0.284373 0.476368 11.00000 -1.20000 AFIX 0 C29 1 0.619233 0.236209 0.373148 11.00000 0.04116 0.04575 = 0.03886 0.01822 0.01723 0.00636 AFIX 43 H29 2 0.663253 0.247851 0.337203 11.00000 -1.20000 AFIX 0 C30 1 0.544577 0.197754 0.343656 11.00000 0.05002 0.04466 = 0.03476 -0.00427 0.01880 -0.00443 AFIX 43 H30 2 0.537121 0.182723 0.286846 11.00000 -1.20000 AFIX 0 C31 1 0.479373 0.180328 0.395695 11.00000 0.04327 0.03906 = 0.03901 -0.00830 0.01489 -0.01028 AFIX 43 H31 2 0.427164 0.154009 0.373944 11.00000 -1.20000 AFIX 0 C32 1 0.481343 0.115922 0.585609 11.00000 0.02746 0.03128 = 0.02268 0.00892 0.00887 0.00976 C33 1 0.589336 0.118779 0.639267 11.00000 0.03440 0.03378 = 0.04228 0.00051 0.00963 0.00578 AFIX 43 H33 2 0.622504 0.151365 0.654632 11.00000 -1.20000 AFIX 0 C34 1 0.648342 0.075222 0.670171 11.00000 0.04146 0.05610 = 0.03272 0.00362 0.00478 0.01702 AFIX 43 H34 2 0.721307 0.078033 0.707400 11.00000 -1.20000 AFIX 0 C35 1 0.602322 0.027046 0.647497 11.00000 0.04654 0.05089 = 0.04334 0.01491 0.01588 0.02119 AFIX 43 H35 2 0.643834 -0.003015 0.668010 11.00000 -1.20000 AFIX 0 C36 1 0.495838 0.023483 0.594946 11.00000 0.05336 0.02674 = 0.06374 0.00616 0.02920 0.00555 AFIX 43 H36 2 0.462769 -0.009129 0.579658 11.00000 -1.20000 AFIX 0 C37 1 0.436105 0.068558 0.563924 11.00000 0.03683 0.03306 = 0.04067 0.00123 0.01499 0.00362 AFIX 43 H37 2 0.362870 0.065911 0.527175 11.00000 -1.20000 AFIX 0 C38 1 0.435584 0.215316 0.647276 11.00000 0.03094 0.03746 = 0.02304 0.00058 0.00134 0.00072 AFIX 23 H38A 2 0.501499 0.201968 0.691816 11.00000 -1.20000 H38B 2 0.451341 0.250733 0.631923 11.00000 -1.20000 AFIX 0 C39 1 0.339636 0.216030 0.688188 11.00000 0.03100 0.03244 = 0.01827 -0.00128 0.00224 0.00310 AFIX 23 H39A 2 0.352713 0.241237 0.737457 11.00000 -1.20000 H39B 2 0.328923 0.181796 0.711654 11.00000 -1.20000 AFIX 0 C40 1 0.093529 0.227808 0.626908 11.00000 0.03521 0.02776 = 0.01919 0.00059 0.00391 0.00042 AFIX 23 H40A 2 0.089821 0.193895 0.654271 11.00000 -1.20000 H40B 2 0.088240 0.254724 0.670136 11.00000 -1.20000 AFIX 0 C41 1 0.000601 0.233511 0.540090 11.00000 0.03040 0.03684 = 0.02686 -0.00125 0.00347 0.00514 AFIX 23 H41A 2 -0.001342 0.269284 0.518644 11.00000 -1.20000 H41B 2 -0.070013 0.226290 0.552196 11.00000 -1.20000 AFIX 0 C42 1 -0.060833 0.222741 0.351004 11.00000 0.02962 0.03413 = 0.02670 0.00178 0.00764 0.00865 C43 1 -0.038251 0.273576 0.337309 11.00000 0.03754 0.02953 = 0.03772 -0.00215 0.00611 0.00735 AFIX 43 H43 2 0.017737 0.290934 0.380887 11.00000 -1.20000 AFIX 0 C44 1 -0.096281 0.299469 0.260834 11.00000 0.05488 0.03764 = 0.04200 0.00701 0.01158 0.01431 AFIX 43 H44 2 -0.080581 0.334431 0.252899 11.00000 -1.20000 AFIX 0 C45 1 -0.176352 0.274611 0.196636 11.00000 0.04575 0.05294 = 0.03145 0.01252 0.00960 0.02719 AFIX 43 H45 2 -0.217256 0.292618 0.145099 11.00000 -1.20000 AFIX 0 C46 1 -0.197253 0.223677 0.207009 11.00000 0.04365 0.06173 = 0.02426 -0.00308 -0.00115 0.00821 AFIX 43 H46 2 -0.250591 0.206126 0.161550 11.00000 -1.20000 AFIX 0 C47 1 -0.140497 0.197934 0.283799 11.00000 0.03895 0.04427 = 0.02817 0.00036 0.00563 0.01062 AFIX 43 H47 2 -0.156066 0.162850 0.290800 11.00000 -1.20000 AFIX 0 C48 1 -0.070563 0.134746 0.457134 11.00000 0.03003 0.04126 = 0.02277 0.00386 0.00374 -0.00026 C49 1 -0.041313 0.085433 0.440575 11.00000 0.03379 0.03232 = 0.04390 -0.00153 0.00898 -0.00518 AFIX 43 H49 2 0.026053 0.079944 0.427394 11.00000 -1.20000 AFIX 0 C50 1 -0.107903 0.044100 0.442808 11.00000 0.04424 0.04008 = 0.04819 0.00296 0.00315 0.00225 AFIX 43 H50 2 -0.086833 0.010589 0.430658 11.00000 -1.20000 AFIX 0 C51 1 -0.205142 0.051779 0.462778 11.00000 0.04452 0.04835 = 0.04832 0.00115 0.00503 -0.01361 AFIX 43 H51 2 -0.250445 0.023339 0.465710 11.00000 -1.20000 AFIX 0 C52 1 -0.236813 0.099995 0.478380 11.00000 0.03643 0.06456 = 0.05104 0.00039 0.01916 -0.01265 AFIX 43 H52 2 -0.304068 0.104945 0.492015 11.00000 -1.20000 AFIX 0 C53 1 -0.171385 0.141719 0.474428 11.00000 0.03215 0.04965 = 0.03819 0.00070 0.00688 0.00047 AFIX 43 H53 2 -0.195047 0.175267 0.483503 11.00000 -1.20000 AFIX 0 C54 1 0.194999 0.123915 0.562925 11.00000 0.03113 0.01970 = 0.03104 -0.00600 0.00494 -0.00495 O1 3 0.181680 0.093633 0.613228 11.00000 0.03901 0.04366 = 0.04414 0.01209 0.00972 0.00525 C55 1 0.207036 0.118587 0.393327 11.00000 0.03272 0.03075 = 0.02756 0.00161 0.00622 0.00619 O2 3 0.207690 0.086159 0.344236 11.00000 0.05688 0.04149 = 0.03704 -0.01204 0.01528 -0.00402 CL 6 0.220124 0.233088 0.356752 11.00000 0.04233 0.03324 = 0.02220 0.00218 0.00786 0.00113 HKLF 4 REM ljh117 in P2(1)/c REM R1 = 0.0408 for 6049 Fo > 4sig(Fo) and 0.0589 for all 7730 data REM 594 parameters refined using 0 restraints END WGHT 0.0455 0.0000 REM Highest difference peak 2.240, deepest hole -1.306, 1-sigma level 0.107 Q1 1 0.2127 0.1298 0.4805 11.00000 0.05 2.24 Q2 1 0.2130 0.2148 0.4806 11.00000 0.05 2.09 Q3 1 0.2145 0.1730 0.4183 11.00000 0.05 1.07 Q4 1 0.2110 0.1725 0.5426 11.00000 0.05 0.99 Q5 1 0.2271 0.2306 0.5360 11.00000 0.05 0.74 Q6 1 0.1219 0.1558 0.4815 11.00000 0.05 0.60 Q7 1 0.2945 0.1916 0.4946 11.00000 0.05 0.53 Q8 1 0.4034 0.1302 0.5559 11.00000 0.05 0.52 Q9 1 0.2838 0.1131 0.5408 11.00000 0.05 0.50 Q10 1 0.0151 0.1456 0.4559 11.00000 0.05 0.50 ; _shelx_res_checksum 15206 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Re Re 0.21067(2) 0.17275(2) 0.47918(2) 0.02352(9) Uani 1 1 d . . B B 0.2871(6) 0.5785(3) 0.5233(4) 0.0367(16) Uani 1 1 d . . N1 N 0.3779(4) 0.5444(2) 0.5920(3) 0.0364(12) Uani 1 1 d . . N2 N 0.1933(4) 0.53935(19) 0.4761(3) 0.0345(12) Uani 1 1 d . . C1 C 0.4758(5) 0.5607(3) 0.6434(4) 0.0423(16) Uani 1 1 d . . C2 C 0.5353(5) 0.5187(3) 0.6911(4) 0.0430(17) Uani 1 1 d . . C3 C 0.4706(5) 0.4754(3) 0.6695(4) 0.0400(15) Uani 1 1 d . . C4 C 0.3712(5) 0.4919(2) 0.6059(3) 0.0331(14) Uani 1 1 d . . C5 C 0.2794(5) 0.4636(2) 0.5582(3) 0.0333(14) Uani 1 1 d . . C6 C 0.1949(4) 0.4865(2) 0.4938(3) 0.0263(12) Uani 1 1 d . . C7 C 0.0953(5) 0.4646(2) 0.4380(4) 0.0330(14) Uani 1 1 d . . C8 C 0.0399(5) 0.5039(3) 0.3853(4) 0.0375(15) Uani 1 1 d . . C9 C 0.1013(5) 0.5494(2) 0.4096(4) 0.0372(15) Uani 1 1 d . . C10 C 0.5141(5) 0.6138(3) 0.6513(5) 0.0551(19) Uani 1 1 d . . H10A H 0.4785 0.6323 0.5962 0.083 Uiso 1 1 calc R U H10B H 0.5935 0.6143 0.6614 0.083 Uiso 1 1 calc R U H10C H 0.4960 0.6302 0.7017 0.083 Uiso 1 1 calc R U C11 C 0.6475(5) 0.5218(3) 0.7540(4) 0.0522(19) Uani 1 1 d . . H11A H 0.6579 0.4928 0.7965 0.063 Uiso 1 1 calc R U H11B H 0.6539 0.5539 0.7889 0.063 Uiso 1 1 calc R U C12 C 0.7381(5) 0.5205(4) 0.7083(4) 0.067(2) Uani 1 1 d . . H12A H 0.8087 0.5264 0.7526 0.100 Uiso 1 1 calc R U H12B H 0.7250 0.5472 0.6624 0.100 Uiso 1 1 calc R U H12C H 0.7388 0.4869 0.6804 0.100 Uiso 1 1 calc R U C13 C 0.4987(5) 0.4233(3) 0.7085(4) 0.0484(18) Uani 1 1 d . . H13A H 0.5761 0.4224 0.7426 0.073 Uiso 1 1 calc R U H13B H 0.4849 0.3979 0.6603 0.073 Uiso 1 1 calc R U H13C H 0.4536 0.4155 0.7481 0.073 Uiso 1 1 calc R U C14 C 0.0559(5) 0.4105(3) 0.4310(4) 0.0433(16) Uani 1 1 d . . H14A H -0.0223 0.4096 0.3994 0.065 Uiso 1 1 calc R U H14B H 0.0679 0.3962 0.4910 0.065 Uiso 1 1 calc R U H14C H 0.0962 0.3902 0.3981 0.065 Uiso 1 1 calc R U C15 C -0.0655(5) 0.4998(3) 0.3116(4) 0.0439(16) Uani 1 1 d . . H15A H -0.0992 0.5341 0.3000 0.053 Uiso 1 1 calc R U H15B H -0.1163 0.4773 0.3319 0.053 Uiso 1 1 calc R U C16 C -0.0520(5) 0.4787(3) 0.2252(4) 0.0527(19) Uani 1 1 d . . H16A H -0.1233 0.4778 0.1801 0.079 Uiso 1 1 calc R U H16B H -0.0221 0.4439 0.2352 0.079 Uiso 1 1 calc R U H16C H -0.0020 0.5007 0.2044 0.079 Uiso 1 1 calc R U C17 C 0.0718(6) 0.6008(3) 0.3686(5) 0.0537(18) Uani 1 1 d . . H17A H 0.1254 0.6261 0.4008 0.081 Uiso 1 1 calc R U H17B H -0.0011 0.6103 0.3722 0.081 Uiso 1 1 calc R U H17C H 0.0718 0.5997 0.3059 0.081 Uiso 1 1 calc R U C18 C 0.3424(5) 0.6016(3) 0.4499(4) 0.0491(17) Uani 1 1 d . . H18A H 0.3850 0.5748 0.4313 0.074 Uiso 1 1 calc R U H18B H 0.3905 0.6302 0.4762 0.074 Uiso 1 1 calc R U H18C H 0.2849 0.6138 0.3978 0.074 Uiso 1 1 calc R U C19 C 0.2389(5) 0.6188(3) 0.5803(4) 0.0458(17) Uani 1 1 d . . H19A H 0.2077 0.6002 0.6218 0.069 Uiso 1 1 calc R U H19B H 0.1819 0.6395 0.5398 0.069 Uiso 1 1 calc R U H19C H 0.2978 0.6412 0.6141 0.069 Uiso 1 1 calc R U C20 C 0.2743(4) 0.4081(2) 0.5731(3) 0.0318(13) Uani 1 1 d . . C21 C 0.3009(5) 0.3734(2) 0.5151(4) 0.0357(14) Uani 1 1 d . . H21 H 0.3307 0.3858 0.4698 0.043 Uiso 1 1 calc R U C22 C 0.2851(5) 0.3217(2) 0.5218(3) 0.0337(14) Uani 1 1 d . . H22 H 0.3036 0.2988 0.4811 0.040 Uiso 1 1 calc R U C23 C 0.2420(4) 0.3025(2) 0.5884(3) 0.0282(13) Uani 1 1 d . . C24 C 0.2236(5) 0.3370(2) 0.6509(3) 0.0337(14) Uani 1 1 d . . H24 H 0.1998 0.3245 0.6993 0.040 Uiso 1 1 calc R U C25 C 0.2394(5) 0.3890(2) 0.6434(4) 0.0334(14) Uani 1 1 d . . H25 H 0.2264 0.4119 0.6866 0.040 Uiso 1 1 calc R U P1 P 0.40512(11) 0.17473(6) 0.54507(8) 0.0249(3) Uani 1 1 d . . P2 P 0.22112(11) 0.23424(6) 0.59690(8) 0.0246(3) Uani 1 1 d . . P3 P 0.01767(11) 0.18928(6) 0.45130(9) 0.0276(3) Uani 1 1 d . . C26 C 0.4910(4) 0.2016(2) 0.4796(3) 0.0285(13) Uani 1 1 d . . C27 C 0.5657(5) 0.2409(3) 0.5081(4) 0.0411(16) Uani 1 1 d . . H27 H 0.5733 0.2566 0.5644 0.049 Uiso 1 1 calc R U C28 C 0.6295(5) 0.2577(3) 0.4554(4) 0.0416(16) Uani 1 1 d . . H28 H 0.6811 0.2844 0.4764 0.050 Uiso 1 1 calc R U C29 C 0.6192(5) 0.2362(3) 0.3731(4) 0.0407(16) Uani 1 1 d . . H29 H 0.6633 0.2479 0.3372 0.049 Uiso 1 1 calc R U C30 C 0.5446(5) 0.1978(3) 0.3437(4) 0.0418(16) Uani 1 1 d . . H30 H 0.5371 0.1827 0.2868 0.050 Uiso 1 1 calc R U C31 C 0.4794(5) 0.1803(2) 0.3957(4) 0.0398(15) Uani 1 1 d . . H31 H 0.4272 0.1540 0.3739 0.048 Uiso 1 1 calc R U C32 C 0.4813(4) 0.1159(2) 0.5856(3) 0.0268(13) Uani 1 1 d . . C33 C 0.5893(5) 0.1188(3) 0.6393(4) 0.0371(15) Uani 1 1 d . . H33 H 0.6225 0.1514 0.6546 0.045 Uiso 1 1 calc R U C34 C 0.6483(5) 0.0752(3) 0.6702(4) 0.0446(17) Uani 1 1 d . . H34 H 0.7213 0.0780 0.7074 0.054 Uiso 1 1 calc R U C35 C 0.6023(5) 0.0270(3) 0.6475(4) 0.0463(17) Uani 1 1 d . . H35 H 0.6438 -0.0030 0.6680 0.056 Uiso 1 1 calc R U C36 C 0.4958(5) 0.0235(3) 0.5949(4) 0.0454(16) Uani 1 1 d . . H36 H 0.4628 -0.0091 0.5797 0.054 Uiso 1 1 calc R U C37 C 0.4361(5) 0.0686(2) 0.5639(4) 0.0360(14) Uani 1 1 d . . H37 H 0.3629 0.0659 0.5272 0.043 Uiso 1 1 calc R U C38 C 0.4356(4) 0.2153(2) 0.6473(3) 0.0318(14) Uani 1 1 d . . H38A H 0.5015 0.2020 0.6918 0.038 Uiso 1 1 calc R U H38B H 0.4513 0.2507 0.6319 0.038 Uiso 1 1 calc R U C39 C 0.3396(4) 0.2160(2) 0.6882(3) 0.0282(13) Uani 1 1 d . . H39A H 0.3527 0.2412 0.7375 0.034 Uiso 1 1 calc R U H39B H 0.3289 0.1818 0.7117 0.034 Uiso 1 1 calc R U C40 C 0.0935(4) 0.2278(2) 0.6269(3) 0.0282(13) Uani 1 1 d . . H40A H 0.0898 0.1939 0.6543 0.034 Uiso 1 1 calc R U H40B H 0.0882 0.2547 0.6701 0.034 Uiso 1 1 calc R U C41 C 0.0006(4) 0.2335(2) 0.5401(3) 0.0323(14) Uani 1 1 d . . H41A H -0.0013 0.2693 0.5186 0.039 Uiso 1 1 calc R U H41B H -0.0700 0.2263 0.5522 0.039 Uiso 1 1 calc R U C42 C -0.0608(4) 0.2227(2) 0.3510(3) 0.0302(13) Uani 1 1 d . . C43 C -0.0383(5) 0.2736(2) 0.3373(4) 0.0359(14) Uani 1 1 d . . H43 H 0.0177 0.2909 0.3809 0.043 Uiso 1 1 calc R U C44 C -0.0963(5) 0.2995(3) 0.2608(4) 0.0453(16) Uani 1 1 d . . H44 H -0.0806 0.3344 0.2529 0.054 Uiso 1 1 calc R U C45 C -0.1764(5) 0.2746(3) 0.1966(4) 0.0437(17) Uani 1 1 d . . H45 H -0.2173 0.2926 0.1451 0.052 Uiso 1 1 calc R U C46 C -0.1973(5) 0.2237(3) 0.2070(4) 0.0454(17) Uani 1 1 d . . H46 H -0.2506 0.2061 0.1615 0.055 Uiso 1 1 calc R U C47 C -0.1405(5) 0.1979(3) 0.2838(3) 0.0379(15) Uani 1 1 d . . H47 H -0.1561 0.1629 0.2908 0.046 Uiso 1 1 calc R U C48 C -0.0706(4) 0.1347(2) 0.4571(3) 0.0321(14) Uani 1 1 d . . C49 C -0.0413(5) 0.0854(2) 0.4406(4) 0.0371(14) Uani 1 1 d . . H49 H 0.0261 0.0799 0.4274 0.045 Uiso 1 1 calc R U C50 C -0.1079(5) 0.0441(3) 0.4428(4) 0.0462(17) Uani 1 1 d . . H50 H -0.0868 0.0106 0.4307 0.055 Uiso 1 1 calc R U C51 C -0.2051(5) 0.0518(3) 0.4628(4) 0.0488(17) Uani 1 1 d . . H51 H -0.2504 0.0233 0.4657 0.059 Uiso 1 1 calc R U C52 C -0.2368(5) 0.1000(3) 0.4784(4) 0.0493(18) Uani 1 1 d . . H52 H -0.3041 0.1049 0.4920 0.059 Uiso 1 1 calc R U C53 C -0.1714(5) 0.1417(3) 0.4744(4) 0.0406(16) Uani 1 1 d . . H53 H -0.1950 0.1753 0.4835 0.049 Uiso 1 1 calc R U C54 C 0.1950(4) 0.1239(2) 0.5629(4) 0.0281(13) Uani 1 1 d . . O1 O 0.1817(3) 0.09363(17) 0.6132(3) 0.0427(11) Uani 1 1 d . . C55 C 0.2070(4) 0.1186(2) 0.3933(4) 0.0308(13) Uani 1 1 d . . O2 O 0.2077(3) 0.08616(18) 0.3442(3) 0.0447(11) Uani 1 1 d . . Cl Cl 0.22012(11) 0.23309(6) 0.35675(8) 0.0329(3) Uani 1 1 d . . 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 Re 0.02648(14) 0.02370(15) 0.01895(13) -0.00037(11) 0.00415(9) 0.00130(12) B 0.041(4) 0.030(4) 0.038(4) -0.004(3) 0.010(3) -0.008(4) N1 0.043(3) 0.032(3) 0.034(3) -0.008(2) 0.011(2) -0.006(3) N2 0.042(3) 0.026(3) 0.036(3) -0.003(2) 0.012(2) 0.001(2) C1 0.045(4) 0.043(4) 0.040(3) -0.014(3) 0.014(3) -0.006(3) C2 0.042(4) 0.059(5) 0.030(3) -0.012(3) 0.013(3) -0.008(4) C3 0.044(4) 0.046(4) 0.029(3) -0.004(3) 0.010(3) 0.003(3) C4 0.037(3) 0.034(4) 0.027(3) -0.006(3) 0.007(3) -0.003(3) C5 0.048(4) 0.030(4) 0.024(3) -0.006(3) 0.013(3) -0.003(3) C6 0.032(3) 0.015(3) 0.026(3) 0.003(2) 0.001(2) -0.005(3) C7 0.041(3) 0.029(4) 0.031(3) 0.000(3) 0.012(3) 0.000(3) C8 0.042(4) 0.035(4) 0.036(3) 0.001(3) 0.012(3) 0.000(3) C9 0.044(4) 0.035(4) 0.034(3) 0.001(3) 0.013(3) 0.002(3) C10 0.050(4) 0.060(5) 0.056(4) -0.021(4) 0.015(3) -0.018(4) C11 0.041(4) 0.077(6) 0.037(3) -0.010(4) 0.008(3) -0.012(4) C12 0.050(4) 0.103(7) 0.048(4) -0.029(4) 0.014(3) 0.000(5) C13 0.041(4) 0.065(5) 0.035(3) -0.001(3) 0.003(3) 0.007(4) C14 0.038(3) 0.042(4) 0.041(3) 0.002(3) -0.003(3) -0.015(3) C15 0.034(3) 0.052(5) 0.041(3) 0.003(3) 0.004(3) 0.001(3) C16 0.043(4) 0.067(5) 0.042(4) -0.002(4) 0.002(3) -0.005(4) C17 0.059(4) 0.041(5) 0.058(4) 0.013(4) 0.011(4) 0.008(4) C18 0.059(4) 0.038(4) 0.054(4) 0.003(3) 0.022(3) -0.006(4) C19 0.048(4) 0.039(4) 0.053(4) -0.006(3) 0.020(3) -0.005(3) C20 0.034(3) 0.030(4) 0.027(3) 0.001(3) 0.003(2) 0.004(3) C21 0.047(4) 0.031(4) 0.032(3) 0.001(3) 0.016(3) -0.002(3) C22 0.047(3) 0.032(4) 0.026(3) -0.008(3) 0.015(3) -0.002(3) C23 0.030(3) 0.032(4) 0.020(3) 0.003(2) 0.004(2) 0.004(3) C24 0.041(3) 0.038(4) 0.023(3) 0.000(3) 0.010(2) 0.009(3) C25 0.051(4) 0.023(3) 0.028(3) -0.004(3) 0.013(3) 0.007(3) P1 0.0282(7) 0.0224(8) 0.0214(7) -0.0027(6) 0.0026(5) 0.0008(6) P2 0.0299(7) 0.0236(8) 0.0189(7) -0.0005(6) 0.0048(5) 0.0032(6) P3 0.0271(7) 0.0295(9) 0.0240(7) 0.0004(6) 0.0040(6) 0.0039(6) C26 0.027(3) 0.029(3) 0.027(3) 0.005(3) 0.005(2) 0.000(3) C27 0.041(3) 0.046(4) 0.035(3) -0.006(3) 0.008(3) -0.005(3) C28 0.044(4) 0.039(4) 0.046(4) 0.000(3) 0.019(3) -0.014(3) C29 0.041(4) 0.046(4) 0.039(3) 0.018(3) 0.017(3) 0.006(3) C30 0.050(4) 0.045(4) 0.035(3) -0.004(3) 0.019(3) -0.004(3) C31 0.043(4) 0.039(4) 0.039(3) -0.008(3) 0.015(3) -0.010(3) C32 0.027(3) 0.031(4) 0.023(3) 0.009(2) 0.009(2) 0.010(3) C33 0.034(3) 0.034(4) 0.042(3) 0.001(3) 0.010(3) 0.006(3) C34 0.041(4) 0.056(5) 0.033(3) 0.004(3) 0.005(3) 0.017(4) C35 0.047(4) 0.051(5) 0.043(4) 0.015(3) 0.016(3) 0.021(4) C36 0.053(4) 0.027(4) 0.064(4) 0.006(3) 0.029(4) 0.006(3) C37 0.037(3) 0.033(4) 0.041(3) 0.001(3) 0.015(3) 0.004(3) C38 0.031(3) 0.037(4) 0.023(3) 0.001(3) 0.001(2) 0.001(3) C39 0.031(3) 0.032(4) 0.018(3) -0.001(2) 0.002(2) 0.003(3) C40 0.035(3) 0.028(3) 0.019(3) 0.001(2) 0.004(2) 0.000(3) C41 0.030(3) 0.037(4) 0.027(3) -0.001(3) 0.003(2) 0.005(3) C42 0.030(3) 0.034(4) 0.027(3) 0.002(3) 0.008(2) 0.009(3) C43 0.038(3) 0.030(4) 0.038(3) -0.002(3) 0.006(3) 0.007(3) C44 0.055(4) 0.038(4) 0.042(4) 0.007(3) 0.012(3) 0.014(3) C45 0.046(4) 0.053(5) 0.031(3) 0.013(3) 0.010(3) 0.027(4) C46 0.044(4) 0.062(5) 0.024(3) -0.003(3) -0.001(3) 0.008(4) C47 0.039(3) 0.044(4) 0.028(3) 0.000(3) 0.006(3) 0.011(3) C48 0.030(3) 0.041(4) 0.023(3) 0.004(3) 0.004(2) 0.000(3) C49 0.034(3) 0.032(4) 0.044(4) -0.002(3) 0.009(3) -0.005(3) C50 0.044(4) 0.040(4) 0.048(4) 0.003(3) 0.003(3) 0.002(3) C51 0.045(4) 0.048(5) 0.048(4) 0.001(3) 0.005(3) -0.014(4) C52 0.036(4) 0.065(5) 0.051(4) 0.000(4) 0.019(3) -0.013(4) C53 0.032(3) 0.050(5) 0.038(3) 0.001(3) 0.007(3) 0.000(3) C54 0.031(3) 0.020(3) 0.031(3) -0.006(3) 0.005(2) -0.005(3) O1 0.039(2) 0.044(3) 0.044(2) 0.012(2) 0.010(2) 0.005(2) C55 0.033(3) 0.031(4) 0.028(3) 0.002(3) 0.006(2) 0.006(3) O2 0.057(3) 0.041(3) 0.037(2) -0.012(2) 0.015(2) -0.004(2) Cl 0.0423(8) 0.0332(8) 0.0222(6) 0.0022(6) 0.0079(6) 0.0011(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' O O 0.0492 0.0322 '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' 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' Re Re -5.2083 5.8923 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle P1 Re P2 80.37(5) P1 Re P3 161.81(5) P1 Re C54 91.02(17) P1 Re C55 97.51(16) P1 Re Cl 92.61(5) P2 Re P3 81.45(5) P2 Re C54 85.10(17) P2 Re C55 174.63(17) P2 Re Cl 99.16(5) P3 Re C54 86.66(17) P3 Re C55 100.53(16) P3 Re Cl 91.03(5) C54 Re C55 90.0(2) C54 Re Cl 174.82(16) C55 Re Cl 85.84(17) N1 B N2 105.1(5) N1 B C18 107.6(5) N1 B C19 108.0(5) N2 B C18 109.5(5) N2 B C19 108.8(5) C18 B C19 117.3(6) B N1 C1 126.5(6) B N1 C4 125.7(5) C1 N1 C4 107.7(5) B N2 C6 125.0(5) B N2 C9 127.4(5) C6 N2 C9 107.5(5) N1 C1 C2 109.8(6) N1 C1 C10 125.4(6) C2 C1 C10 124.8(6) C1 C2 C3 108.1(6) C1 C2 C11 125.2(7) C3 C2 C11 126.8(7) C2 C3 C4 105.8(6) C2 C3 C13 126.0(6) C4 C3 C13 128.2(6) N1 C4 C3 108.7(5) N1 C4 C5 120.9(5) C3 C4 C5 130.3(6) C4 C5 C6 121.2(6) C4 C5 C20 120.1(5) C6 C5 C20 118.6(5) N2 C6 C5 122.0(5) N2 C6 C7 108.0(5) C5 C6 C7 129.9(5) C6 C7 C8 106.4(5) C6 C7 C14 129.8(5) C8 C7 C14 123.8(5) C7 C8 C9 108.3(5) C7 C8 C15 126.7(6) C9 C8 C15 124.9(6) N2 C9 C8 109.7(6) N2 C9 C17 124.2(6) C8 C9 C17 126.1(6) C1 C10 H10A 109.5 C1 C10 H10B 109.5 C1 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C2 C11 H11A 108.8 C2 C11 H11B 108.8 C2 C11 C12 113.8(5) H11A C11 H11B 107.7 H11A C11 C12 108.8 H11B C11 C12 108.8 C11 C12 H12A 109.5 C11 C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C3 C13 H13A 109.5 C3 C13 H13B 109.5 C3 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C7 C14 H14A 109.5 C7 C14 H14B 109.5 C7 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C8 C15 H15A 108.8 C8 C15 H15B 108.8 C8 C15 C16 114.0(5) H15A C15 H15B 107.7 H15A C15 C16 108.8 H15B C15 C16 108.8 C15 C16 H16A 109.5 C15 C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C9 C17 H17A 109.5 C9 C17 H17B 109.5 C9 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 B C18 H18A 109.5 B C18 H18B 109.5 B C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 B C19 H19A 109.5 B C19 H19B 109.5 B C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C5 C20 C21 120.6(5) C5 C20 C25 121.0(5) C21 C20 C25 118.4(6) C20 C21 H21 119.3 C20 C21 C22 121.5(5) H21 C21 C22 119.3 C21 C22 H22 119.8 C21 C22 C23 120.4(5) H22 C22 C23 119.8 C22 C23 C24 117.9(6) C22 C23 P2 120.2(4) C24 C23 P2 121.8(4) C23 C24 H24 119.4 C23 C24 C25 121.2(5) H24 C24 C25 119.4 C20 C25 C24 120.4(5) C20 C25 H25 119.8 C24 C25 H25 119.8 Re P1 C26 118.48(17) Re P1 C32 120.84(19) Re P1 C38 108.54(17) C26 P1 C32 99.8(2) C26 P1 C38 104.3(3) C32 P1 C38 102.7(3) Re P2 C23 125.10(17) Re P2 C39 106.04(18) Re P2 C40 105.91(18) C23 P2 C39 102.0(3) C23 P2 C40 105.6(3) C39 P2 C40 112.2(2) Re P3 C41 107.78(17) Re P3 C42 121.55(18) Re P3 C48 117.49(19) C41 P3 C42 101.0(3) C41 P3 C48 103.9(3) C42 P3 C48 102.7(3) P1 C26 C27 124.7(4) P1 C26 C31 116.8(4) C27 C26 C31 118.5(5) C26 C27 H27 119.6 C26 C27 C28 120.8(6) H27 C27 C28 119.6 C27 C28 H28 119.6 C27 C28 C29 120.8(6) H28 C28 C29 119.6 C28 C29 H29 120.5 C28 C29 C30 119.1(5) H29 C29 C30 120.5 C29 C30 H30 119.5 C29 C30 C31 121.1(6) H30 C30 C31 119.5 C26 C31 C30 119.8(6) C26 C31 H31 120.1 C30 C31 H31 120.1 P1 C32 C33 119.9(5) P1 C32 C37 121.8(4) C33 C32 C37 118.2(5) C32 C33 H33 119.5 C32 C33 C34 121.0(6) H33 C33 C34 119.5 C33 C34 H34 119.7 C33 C34 C35 120.6(6) H34 C34 C35 119.7 C34 C35 H35 120.4 C34 C35 C36 119.1(6) H35 C35 C36 120.4 C35 C36 H36 120.2 C35 C36 C37 119.6(6) H36 C36 C37 120.2 C32 C37 C36 121.4(6) C32 C37 H37 119.3 C36 C37 H37 119.3 P1 C38 H38A 109.3 P1 C38 H38B 109.3 P1 C38 C39 111.5(4) H38A C38 H38B 108.0 H38A C38 C39 109.3 H38B C38 C39 109.3 P2 C39 C38 105.1(3) P2 C39 H39A 110.7 P2 C39 H39B 110.7 C38 C39 H39A 110.7 C38 C39 H39B 110.7 H39A C39 H39B 108.8 P2 C40 H40A 110.4 P2 C40 H40B 110.4 P2 C40 C41 106.6(3) H40A C40 H40B 108.6 H40A C40 C41 110.4 H40B C40 C41 110.4 P3 C41 C40 111.9(4) P3 C41 H41A 109.2 P3 C41 H41B 109.2 C40 C41 H41A 109.2 C40 C41 H41B 109.2 H41A C41 H41B 107.9 P3 C42 C43 120.2(4) P3 C42 C47 121.9(5) C43 C42 C47 117.8(5) C42 C43 H43 119.5 C42 C43 C44 121.0(6) H43 C43 C44 119.5 C43 C44 H44 119.9 C43 C44 C45 120.1(7) H44 C44 C45 119.9 C44 C45 H45 120.0 C44 C45 C46 120.0(6) H45 C45 C46 120.0 C45 C46 H46 120.0 C45 C46 C47 120.0(6) H46 C46 C47 120.0 C42 C47 C46 121.0(7) C42 C47 H47 119.5 C46 C47 H47 119.5 P3 C48 C49 120.7(4) P3 C48 C53 121.3(5) C49 C48 C53 117.9(6) C48 C49 H49 119.3 C48 C49 C50 121.4(6) H49 C49 C50 119.3 C49 C50 H50 120.2 C49 C50 C51 119.5(7) H50 C50 C51 120.2 C50 C51 H51 119.8 C50 C51 C52 120.4(7) H51 C51 C52 119.8 C51 C52 H52 119.8 C51 C52 C53 120.3(6) H52 C52 C53 119.8 C48 C53 C52 120.4(7) C48 C53 H53 119.8 C52 C53 H53 119.8 Re C54 O1 177.8(5) Re C55 O2 178.0(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Re P1 2.4012(14) Re P2 2.4157(13) Re P3 2.4147(14) Re C54 1.878(6) Re C55 1.940(6) Re Cl 2.5068(13) B N1 1.605(9) B N2 1.586(8) B C18 1.624(9) B C19 1.609(9) N1 C1 1.347(7) N1 C4 1.395(8) N2 C6 1.407(7) N2 C9 1.354(7) C1 C2 1.417(9) C1 C10 1.463(9) C2 C3 1.385(9) C2 C11 1.491(8) C3 C4 1.437(8) C3 C13 1.491(9) C4 C5 1.405(8) C5 C6 1.384(7) C5 C20 1.472(8) C6 C7 1.438(7) C7 C8 1.378(8) C7 C14 1.493(8) C8 C9 1.412(9) C8 C15 1.506(8) C9 C17 1.488(9) C10 H10A 0.980 C10 H10B 0.980 C10 H10C 0.980 C11 H11A 0.990 C11 H11B 0.990 C11 C12 1.523(8) C12 H12A 0.980 C12 H12B 0.980 C12 H12C 0.980 C13 H13A 0.980 C13 H13B 0.980 C13 H13C 0.980 C14 H14A 0.980 C14 H14B 0.980 C14 H14C 0.980 C15 H15A 0.990 C15 H15B 0.990 C15 C16 1.511(8) C16 H16A 0.980 C16 H16B 0.980 C16 H16C 0.980 C17 H17A 0.980 C17 H17B 0.980 C17 H17C 0.980 C18 H18A 0.980 C18 H18B 0.980 C18 H18C 0.980 C19 H19A 0.980 C19 H19B 0.980 C19 H19C 0.980 C20 C21 1.389(8) C20 C25 1.389(7) C21 H21 0.950 C21 C22 1.375(8) C22 H22 0.950 C22 C23 1.401(7) C23 C24 1.396(7) C23 P2 1.811(6) C24 H24 0.950 C24 C25 1.383(8) C25 H25 0.950 P1 C26 1.837(5) P1 C32 1.831(6) P1 C38 1.863(5) P2 C39 1.822(5) P2 C40 1.826(5) P3 C41 1.864(5) P3 C42 1.824(6) P3 C48 1.833(6) C26 C27 1.385(8) C26 C31 1.393(8) C27 H27 0.950 C27 C28 1.383(8) C28 H28 0.950 C28 C29 1.374(8) C29 H29 0.950 C29 C30 1.370(9) C30 H30 0.950 C30 C31 1.394(8) C31 H31 0.950 C32 C33 1.396(7) C32 C37 1.366(8) C33 H33 0.950 C33 C34 1.373(8) C34 H34 0.950 C34 C35 1.390(9) C35 H35 0.950 C35 C36 1.376(9) C36 H36 0.950 C36 C37 1.411(8) C37 H37 0.950 C38 H38A 0.990 C38 H38B 0.990 C38 C39 1.534(7) C39 H39A 0.990 C39 H39B 0.990 C40 H40A 0.990 C40 H40B 0.990 C40 C41 1.534(7) C41 H41A 0.990 C41 H41B 0.990 C42 C43 1.387(8) C42 C47 1.396(8) C43 H43 0.950 C43 C44 1.389(8) C44 H44 0.950 C44 C45 1.374(9) C45 H45 0.950 C45 C46 1.375(9) C46 H46 0.950 C46 C47 1.386(8) C47 H47 0.950 C48 C49 1.385(8) C48 C53 1.400(8) C49 H49 0.950 C49 C50 1.380(8) C50 H50 0.950 C50 C51 1.377(9) C51 H51 0.950 C51 C52 1.365(10) C52 H52 0.950 C52 C53 1.384(9) C53 H53 0.950 C54 O1 1.161(6) C55 O2 1.144(7) 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 N2 B N1 C1 175.8(5) N2 B N1 C4 -0.9(7) C18 B N1 C1 59.3(7) C18 B N1 C4 -117.5(6) C19 B N1 C1 -68.2(7) C19 B N1 C4 115.0(6) N1 B N2 C6 -0.2(7) N1 B N2 C9 -176.5(5) C18 B N2 C6 115.1(6) C18 B N2 C9 -61.3(7) C19 B N2 C6 -115.6(6) C19 B N2 C9 68.0(7) B N1 C1 C2 -176.6(5) B N1 C1 C10 5.2(9) C4 N1 C1 C2 0.6(6) C4 N1 C1 C10 -177.5(6) N1 C1 C2 C3 -1.2(7) N1 C1 C2 C11 179.4(5) C10 C1 C2 C3 177.0(6) C10 C1 C2 C11 -2.4(10) C1 C2 C3 C4 1.2(6) C1 C2 C3 C13 -176.3(6) C11 C2 C3 C4 -179.4(5) C11 C2 C3 C13 3.1(10) B N1 C4 C3 177.4(5) B N1 C4 C5 -0.1(8) C1 N1 C4 C3 0.1(6) C1 N1 C4 C5 -177.3(5) C2 C3 C4 N1 -0.9(6) C2 C3 C4 C5 176.3(6) C13 C3 C4 N1 176.6(5) C13 C3 C4 C5 -6.2(10) N1 C4 C5 C6 2.4(8) N1 C4 C5 C20 179.3(5) C3 C4 C5 C6 -174.5(5) C3 C4 C5 C20 2.5(9) C4 C5 C6 N2 -3.5(8) C4 C5 C6 C7 179.7(5) C20 C5 C6 N2 179.5(5) C20 C5 C6 C7 2.7(9) B N2 C6 C5 2.3(8) B N2 C6 C7 179.7(5) C9 N2 C6 C5 179.3(5) C9 N2 C6 C7 -3.3(6) N2 C6 C7 C8 3.2(6) N2 C6 C7 C14 -179.5(5) C5 C6 C7 C8 -179.7(5) C5 C6 C7 C14 -2.4(10) C6 C7 C8 C9 -1.9(6) C6 C7 C8 C15 175.7(5) C14 C7 C8 C9 -179.4(5) C14 C7 C8 C15 -1.8(9) B N2 C9 C8 179.0(5) B N2 C9 C17 -0.3(9) C6 N2 C9 C8 2.1(6) C6 N2 C9 C17 -177.2(5) C7 C8 C9 N2 -0.1(7) C7 C8 C9 C17 179.2(6) C15 C8 C9 N2 -177.8(5) C15 C8 C9 C17 1.5(10) C1 C2 C11 C12 -82.5(9) C3 C2 C11 C12 98.2(8) C7 C8 C15 C16 -78.2(8) C9 C8 C15 C16 99.1(8) C4 C5 C20 C21 -98.6(7) C4 C5 C20 C25 83.5(7) C6 C5 C20 C21 78.4(7) C6 C5 C20 C25 -99.4(6) C5 C20 C21 C22 -172.7(6) C25 C20 C21 C22 5.3(9) C20 C21 C22 C23 -0.4(9) C21 C22 C23 C24 -4.6(8) C21 C22 C23 P2 179.9(4) C22 C23 C24 C25 4.9(8) P2 C23 C24 C25 -179.8(4) C23 C24 C25 C20 0.0(9) C5 C20 C25 C24 172.9(5) C21 C20 C25 C24 -5.0(9) C22 C23 P2 Re -19.0(5) C22 C23 P2 C39 100.6(5) C22 C23 P2 C40 -142.0(4) C24 C23 P2 Re 165.8(4) C24 C23 P2 C39 -74.6(5) C24 C23 P2 C40 42.8(5) Re P1 C26 C27 125.1(5) Re P1 C26 C31 -55.2(5) C32 P1 C26 C27 -101.7(5) C32 P1 C26 C31 78.1(5) C38 P1 C26 C27 4.3(6) C38 P1 C26 C31 -176.0(5) P1 C26 C27 C28 177.9(5) C31 C26 C27 C28 -1.8(9) C26 C27 C28 C29 0.9(10) C27 C28 C29 C30 0.0(10) C28 C29 C30 C31 0.1(10) P1 C26 C31 C30 -177.9(5) C27 C26 C31 C30 1.8(9) C29 C30 C31 C26 -1.0(10) Re P1 C32 C33 -167.2(3) Re P1 C32 C37 13.7(5) C26 P1 C32 C33 61.0(5) C26 P1 C32 C37 -118.1(5) C38 P1 C32 C33 -46.3(5) C38 P1 C32 C37 134.6(5) P1 C32 C33 C34 -179.7(4) C37 C32 C33 C34 -0.6(8) C32 C33 C34 C35 1.0(9) C33 C34 C35 C36 -1.3(9) C34 C35 C36 C37 1.0(9) P1 C32 C37 C36 179.5(4) C33 C32 C37 C36 0.4(8) C35 C36 C37 C32 -0.6(9) Re P1 C38 C39 26.7(4) C26 P1 C38 C39 153.9(4) C32 P1 C38 C39 -102.3(4) P1 C38 C39 P2 -52.8(5) Re P2 C39 C38 56.0(4) C23 P2 C39 C38 -76.3(4) C40 P2 C39 C38 171.1(4) Re P2 C40 C41 -53.5(4) C23 P2 C40 C41 81.0(4) C39 P2 C40 C41 -168.7(4) P2 C40 C41 P3 52.4(5) Re P3 C41 C40 -27.6(4) C42 P3 C41 C40 -156.0(4) C48 P3 C41 C40 97.8(4) Re P3 C42 C43 -65.1(5) Re P3 C42 C47 111.4(4) C41 P3 C42 C43 53.9(5) C41 P3 C42 C47 -129.7(5) C48 P3 C42 C43 161.0(5) C48 P3 C42 C47 -22.5(5) P3 C42 C43 C44 179.2(4) C47 C42 C43 C44 2.6(8) C42 C43 C44 C45 -1.0(9) C43 C44 C45 C46 -1.6(9) C44 C45 C46 C47 2.5(9) C45 C46 C47 C42 -0.8(9) P3 C42 C47 C46 -178.3(4) C43 C42 C47 C46 -1.7(8) Re P3 C48 C49 -26.4(5) Re P3 C48 C53 156.5(4) C41 P3 C48 C49 -145.3(5) C41 P3 C48 C53 37.5(5) C42 P3 C48 C49 109.8(5) C42 P3 C48 C53 -67.3(5) P3 C48 C49 C50 -178.6(4) C53 C48 C49 C50 -1.4(9) C48 C49 C50 C51 -0.7(9) C49 C50 C51 C52 1.4(10) C50 C51 C52 C53 -0.1(10) C51 C52 C53 C48 -2.0(9) P3 C48 C53 C52 179.9(4) C49 C48 C53 C52 2.7(8)