#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238974.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_2238974 loop_ _publ_author_name 'Pawar, Gajanan Manohar' 'Wurst, Klaus' 'Wang, Dongren' 'Buchmeiser, Michael' _publ_section_title ; [\m-3,3'-Diisopropyl-1,1'-(propane-1,3-diyl)bis(1,3-diazinan-2-ylidene)]bis[bromido(\h^4^-cycloocta-1,5-diene)rhodium(I)] ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m71 _journal_page_last m72 _journal_paper_doi 10.1107/S1600536814001135 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac '[Rh2 Br2 (C8 H12)2 (C17 H32 N4)]' _chemical_formula_moiety 'C33 H56 Br2 N4 Rh2' _chemical_formula_sum 'C33 H56 Br2 N4 Rh2' _chemical_formula_weight 874.46 _chemical_name_systematic '[\m-3,3'-Diisopropyl-1,1'-(propane-1,3-diyl)bis(1,3-diazinan-2-ylidene)]bis[bromido(\h^4^-cycloocta-1,5-diene)rhodium(I)]' _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 16.4075(2) _cell_length_b 15.7975(3) _cell_length_c 27.1065(4) _cell_measurement_reflns_used 54150 _cell_measurement_temperature 233(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 1.0 _cell_volume 7025.94(19) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS86 (Sheldrick, 2008)' _diffrn_ambient_temperature 233(2) _diffrn_detector_area_resol_mean 9.1 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 57878 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.94 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.242 _exptl_absorpt_correction_T_max 0.755 _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SORTAV; Blessing, 1995) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 3536 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.953 _refine_diff_density_min -0.513 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 402 _refine_ls_number_reflns 6186 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0333 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+11.9446P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.0776 _reflns_number_gt 5045 _reflns_number_total 6186 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL p in Pbca CELL 0.71073 16.4075 15.7975 27.1065 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0003 0.0004 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N BR RH UNIT 264 448 32 16 16 ACTA L.S. 6 TEMP -40 OMIT -3 50 FMAP 2 PLAN 10 BOND 0.5 DFIX 0.93 0.02 C1 H1 C2 H2 C5 H5 C6 H6 C9 H9 C10 H10 C13 H13 C14 H14 BOND $H WGHT 0.025400 11.944599 FVAR 0.10865 RH1 5 0.311925 0.057582 0.871181 11.00000 0.02475 0.02505 = 0.03142 0.00325 -0.00464 -0.00038 RH2 5 0.322674 0.166937 0.624003 11.00000 0.02445 0.02526 = 0.02930 0.00182 0.00006 0.00086 BR1 4 0.215909 0.182327 0.873742 11.00000 0.03851 0.03332 = 0.05199 -0.00114 -0.00447 0.00655 BR2 4 0.233325 0.038520 0.613041 11.00000 0.04445 0.03300 = 0.06797 -0.00436 -0.00333 -0.00669 N1 3 0.171687 -0.062339 0.875240 11.00000 0.03515 0.02785 = 0.03065 0.00248 -0.00366 -0.00846 N4 3 0.175950 0.277940 0.613819 11.00000 0.02899 0.03386 = 0.03200 0.00061 -0.00164 0.00624 N2 3 0.206579 -0.021411 0.796274 11.00000 0.03768 0.03628 = 0.02798 0.00364 -0.00544 -0.00689 N3 3 0.206288 0.239753 0.693997 11.00000 0.03219 0.03631 = 0.02724 0.00447 0.00311 0.00761 C1 1 0.398774 -0.028527 0.843937 11.00000 0.03568 0.04059 = 0.06224 -0.00883 0.00074 0.01131 H1 2 0.375544 -0.063673 0.820457 11.00000 0.04961 C2 1 0.379735 -0.049755 0.892456 11.00000 0.04005 0.03091 = 0.06548 0.00754 -0.01723 0.00726 H2 2 0.342100 -0.089966 0.900111 11.00000 0.04142 C3 1 0.434353 -0.030124 0.936028 11.00000 0.09521 0.06634 = 0.07725 0.00775 -0.05120 0.01525 AFIX 21 H3A 2 0.420104 -0.069000 0.962850 11.00000 -1.20000 H3B 2 0.490662 -0.042590 0.926404 11.00000 -1.20000 AFIX 0 C4 1 0.431953 0.055931 0.955506 11.00000 0.10397 0.06069 = 0.07295 0.00301 -0.05076 -0.00323 AFIX 21 H4A 2 0.487641 0.072881 0.964068 11.00000 -1.20000 H4B 2 0.400026 0.055589 0.986061 11.00000 -1.20000 AFIX 0 C5 1 0.396807 0.121427 0.921696 11.00000 0.04681 0.03827 = 0.06052 -0.00547 -0.02482 -0.00385 H5 2 0.360683 0.157948 0.937223 11.00000 0.05923 C6 1 0.421322 0.138549 0.875190 11.00000 0.03457 0.03719 = 0.08052 0.00784 -0.00721 -0.00920 H6 2 0.401358 0.189484 0.862902 11.00000 0.02459 C7 1 0.492401 0.097033 0.849160 11.00000 0.04659 0.07499 = 0.11779 -0.00034 0.02429 -0.01712 AFIX 21 H7A 2 0.511485 0.135278 0.823144 11.00000 -1.20000 H7B 2 0.536981 0.090484 0.872917 11.00000 -1.20000 AFIX 0 C8 1 0.475757 0.014359 0.827012 11.00000 0.04837 0.09016 = 0.10473 -0.00883 0.02590 -0.00047 AFIX 21 H8A 2 0.521834 -0.023167 0.834150 11.00000 -1.20000 H8B 2 0.473021 0.021366 0.791128 11.00000 -1.20000 AFIX 0 C9 1 0.383170 0.279827 0.605244 11.00000 0.03696 0.02804 = 0.06089 0.00080 0.00709 -0.00464 H9 2 0.346204 0.325105 0.602438 11.00000 0.03393 C10 1 0.403475 0.258239 0.653989 11.00000 0.03142 0.05051 = 0.05418 -0.01721 -0.00099 -0.00791 H10 2 0.375630 0.283023 0.680261 11.00000 0.04921 C11 1 0.484958 0.221193 0.669500 11.00000 0.03461 0.08456 = 0.06614 -0.01617 -0.01260 -0.00280 AFIX 21 H11A 2 0.527521 0.243537 0.647734 11.00000 -1.20000 H11B 2 0.497277 0.240061 0.703124 11.00000 -1.20000 AFIX 0 C12 1 0.487839 0.125468 0.668036 11.00000 0.03432 0.08418 = 0.05223 0.01433 -0.00479 0.01227 AFIX 21 H12A 2 0.543771 0.107556 0.660830 11.00000 -1.20000 H12B 2 0.473401 0.103475 0.700692 11.00000 -1.20000 AFIX 0 C13 1 0.431371 0.087029 0.630175 11.00000 0.02734 0.04205 = 0.04911 0.01091 0.00501 0.00926 H13 2 0.408965 0.036983 0.640720 11.00000 0.05323 C14 1 0.425571 0.111609 0.582422 11.00000 0.03401 0.03824 = 0.04336 -0.00351 0.00626 0.00716 H14 2 0.398687 0.075585 0.560445 11.00000 0.03478 C15 1 0.476532 0.180257 0.558931 11.00000 0.04764 0.06313 = 0.04560 0.00859 0.01553 0.00206 AFIX 21 H15A 2 0.487689 0.164950 0.524553 11.00000 -1.20000 H15B 2 0.528854 0.184048 0.576228 11.00000 -1.20000 AFIX 0 C16 1 0.435153 0.265756 0.560276 11.00000 0.05731 0.05177 = 0.06853 0.01654 0.02154 -0.01104 AFIX 21 H16A 2 0.476972 0.309989 0.558938 11.00000 -1.20000 H16B 2 0.400969 0.271612 0.530826 11.00000 -1.20000 AFIX 0 C17 1 0.219501 -0.015822 0.845360 11.00000 0.02785 0.02318 = 0.02947 0.00027 -0.00321 0.00518 C18 1 0.103985 -0.113458 0.856857 11.00000 0.04448 0.04228 = 0.04880 -0.00235 -0.00185 -0.01723 AFIX 21 H18A 2 0.054591 -0.078717 0.855045 11.00000 -1.20000 H18B 2 0.093585 -0.160438 0.879613 11.00000 -1.20000 AFIX 0 C19 1 0.123898 -0.147626 0.806674 11.00000 0.05861 0.03759 = 0.05025 -0.00832 -0.00796 -0.01083 AFIX 21 H19A 2 0.170179 -0.186660 0.808871 11.00000 -1.20000 H19B 2 0.077047 -0.178770 0.793506 11.00000 -1.20000 AFIX 0 C20 1 0.144675 -0.075295 0.773151 11.00000 0.05955 0.04814 = 0.03819 -0.00307 -0.01605 -0.01020 AFIX 21 H20A 2 0.165351 -0.097182 0.741723 11.00000 -1.20000 H20B 2 0.095592 -0.041901 0.766394 11.00000 -1.20000 AFIX 0 C21 1 0.248017 0.037782 0.763319 11.00000 0.03868 0.05121 = 0.02858 0.00952 0.00157 0.00237 AFIX 21 H21A 2 0.270464 0.006287 0.735291 11.00000 -1.20000 H21B 2 0.293710 0.063711 0.781033 11.00000 -1.20000 AFIX 0 C22 1 0.192734 0.107323 0.743961 11.00000 0.03414 0.04689 = 0.03093 0.01103 -0.00120 -0.00237 AFIX 21 H22A 2 0.154497 0.125093 0.769732 11.00000 -1.20000 H22B 2 0.161287 0.086623 0.715690 11.00000 -1.20000 AFIX 0 C23 1 0.246200 0.181941 0.728381 11.00000 0.03419 0.04490 = 0.02728 0.00573 -0.00246 0.00124 AFIX 21 H23A 2 0.262303 0.213613 0.757900 11.00000 -1.20000 H23B 2 0.295938 0.160000 0.712979 11.00000 -1.20000 AFIX 0 C24 1 0.140537 0.291034 0.715017 11.00000 0.04562 0.04642 = 0.03951 -0.00294 0.00847 0.01011 AFIX 21 H24A 2 0.157255 0.313323 0.747204 11.00000 -1.20000 H24B 2 0.091888 0.255990 0.719797 11.00000 -1.20000 AFIX 0 C25 1 0.121386 0.363008 0.680613 11.00000 0.04527 0.03547 = 0.05450 -0.00306 0.00893 0.01299 AFIX 21 H25A 2 0.073045 0.393472 0.692261 11.00000 -1.20000 H25B 2 0.167197 0.402781 0.679673 11.00000 -1.20000 AFIX 0 C26 1 0.106132 0.328001 0.630017 11.00000 0.03876 0.04335 = 0.05202 0.00244 -0.00188 0.01668 AFIX 21 H26A 2 0.057210 0.292420 0.630496 11.00000 -1.20000 H26B 2 0.096824 0.374580 0.606813 11.00000 -1.20000 AFIX 0 C27 1 0.222645 0.234583 0.645423 11.00000 0.02767 0.01992 = 0.03153 0.00576 0.00313 -0.00143 C28 1 0.176588 -0.051424 0.929250 11.00000 0.03997 0.03105 = 0.02840 0.00569 0.00121 -0.00283 AFIX 11 H28 2 0.223422 -0.013649 0.936001 11.00000 -1.20000 AFIX 0 C29 1 0.186451 0.265405 0.559984 11.00000 0.03974 0.04154 = 0.02919 0.00474 -0.00572 0.00469 AFIX 11 H29 2 0.236774 0.231746 0.555368 11.00000 -1.20000 AFIX 0 C281 1 0.192664 -0.134498 0.956192 11.00000 0.06994 0.04396 = 0.04463 0.01547 0.00457 0.00842 AFIX 31 H28A 2 0.241902 -0.160306 0.943304 11.00000 -1.50000 H28B 2 0.146984 -0.172539 0.951245 11.00000 -1.50000 H28C 2 0.199335 -0.123493 0.991165 11.00000 -1.50000 AFIX 0 C282 1 0.100632 -0.007183 0.948421 11.00000 0.05142 0.04772 = 0.04786 0.00300 0.00833 0.00761 AFIX 31 H28D 2 0.092526 0.045250 0.930457 11.00000 -1.50000 H28E 2 0.107214 0.005086 0.983257 11.00000 -1.50000 H28F 2 0.053697 -0.043660 0.943781 11.00000 -1.50000 AFIX 0 C291 1 0.198026 0.347459 0.532223 11.00000 0.09532 0.05119 = 0.04100 0.01450 -0.00439 0.00426 AFIX 31 H29A 2 0.243671 0.378270 0.546178 11.00000 -1.50000 H29B 2 0.148992 0.381450 0.534908 11.00000 -1.50000 H29C 2 0.208846 0.335338 0.497759 11.00000 -1.50000 AFIX 0 C292 1 0.116581 0.213630 0.539022 11.00000 0.05418 0.06445 = 0.05034 -0.00237 -0.01719 -0.00598 AFIX 31 H29D 2 0.111151 0.161424 0.557571 11.00000 -1.50000 H29E 2 0.127563 0.200561 0.504695 11.00000 -1.50000 H29F 2 0.066400 0.245833 0.541411 11.00000 -1.50000 HKLF 4 REM p in Pbca REM R1 = 0.0333 for 5045 Fo > 4sig(Fo) and 0.0469 for all 6186 data REM 402 parameters refined using 8 restraints END WGHT 0.0254 11.9446 REM Highest difference peak 0.953, deepest hole -0.513, 1-sigma level 0.083 Q1 1 0.1871 0.2142 0.6273 11.00000 0.05 0.95 Q2 1 0.1783 0.1043 0.8745 11.00000 0.05 0.82 Q3 1 0.2692 0.2324 0.8900 11.00000 0.05 0.45 Q4 1 0.4954 -0.0008 0.8581 11.00000 0.05 0.44 Q5 1 0.2655 0.0555 0.5867 11.00000 0.05 0.41 Q6 1 0.2814 0.0912 0.6265 11.00000 0.05 0.39 Q7 1 0.5362 0.1324 0.8425 11.00000 0.05 0.35 Q8 1 0.3246 0.0030 0.9402 11.00000 0.05 0.34 Q9 1 0.2028 -0.0175 0.8213 11.00000 0.05 0.30 Q10 1 0.2200 0.0966 0.8380 11.00000 0.05 0.30 ; _cod_data_source_file im2446sup1.cf _cod_data_source_block I _cod_database_code 2238974 _cod_database_fobs_code 2238974 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity Rh Rh1 0.311925(16) 0.057582(18) 0.871181(10) 0.02707(9) Uani d . 1 1 Rh Rh2 0.322674(16) 0.166937(18) 0.624003(10) 0.02634(9) Uani d . 1 1 Br Br1 0.21591(3) 0.18233(3) 0.873742(16) 0.04127(12) Uani d . 1 1 Br Br2 0.23333(3) 0.03852(3) 0.613041(18) 0.04847(13) Uani d . 1 1 N N1 0.17169(18) -0.06234(19) 0.87524(11) 0.0312(7) Uani d . 1 1 N N4 0.17595(18) 0.2779(2) 0.61382(11) 0.0316(7) Uani d . 1 1 N N2 0.20658(19) -0.0214(2) 0.79627(11) 0.0340(8) Uani d . 1 1 N N3 0.20629(18) 0.2398(2) 0.69400(11) 0.0319(7) Uani d . 1 1 C C1 0.3988(3) -0.0285(3) 0.84394(18) 0.0462(11) Uani d D 1 1 H H1 0.376(2) -0.064(2) 0.8205(12) 0.050(13) Uiso d D 1 1 C C2 0.3797(3) -0.0498(3) 0.89246(18) 0.0455(11) Uani d D 1 1 H H2 0.3421(19) -0.090(2) 0.9001(15) 0.041(12) Uiso d D 1 1 C C3 0.4344(4) -0.0301(4) 0.9360(2) 0.0796(18) Uani d . 1 1 H H3A 0.4201 -0.0690 0.9628 0.096 Uiso calc . 1 1 H H3B 0.4907 -0.0426 0.9264 0.096 Uiso calc . 1 1 C C4 0.4320(4) 0.0559(4) 0.9555(2) 0.0792(18) Uani d . 1 1 H H4A 0.4876 0.0729 0.9641 0.095 Uiso calc . 1 1 H H4B 0.4000 0.0556 0.9861 0.095 Uiso calc . 1 1 C C5 0.3968(3) 0.1214(3) 0.92170(19) 0.0485(12) Uani d D 1 1 H H5 0.361(2) 0.158(2) 0.9372(15) 0.059(15) Uiso d D 1 1 C C6 0.4213(3) 0.1385(3) 0.8752(2) 0.0508(12) Uani d D 1 1 H H6 0.401(2) 0.1895(15) 0.8629(12) 0.025(9) Uiso d D 1 1 C C7 0.4924(3) 0.0970(4) 0.8492(3) 0.0798(18) Uani d . 1 1 H H7A 0.5115 0.1353 0.8231 0.096 Uiso calc . 1 1 H H7B 0.5370 0.0905 0.8729 0.096 Uiso calc . 1 1 C C8 0.4758(3) 0.0144(4) 0.8270(2) 0.0811(18) Uani d . 1 1 H H8A 0.5218 -0.0232 0.8342 0.097 Uiso calc . 1 1 H H8B 0.4730 0.0214 0.7911 0.097 Uiso calc . 1 1 C C9 0.3832(3) 0.2798(3) 0.60524(17) 0.0420(10) Uani d D 1 1 H H9 0.3462(19) 0.3251(18) 0.6024(14) 0.034(11) Uiso d D 1 1 C C10 0.4035(2) 0.2582(3) 0.65399(18) 0.0454(11) Uani d D 1 1 H H10 0.376(2) 0.283(2) 0.6803(11) 0.049(13) Uiso d D 1 1 C C11 0.4850(3) 0.2212(4) 0.66950(19) 0.0618(14) Uani d . 1 1 H H11A 0.5275 0.2435 0.6477 0.074 Uiso calc . 1 1 H H11B 0.4973 0.2401 0.7031 0.074 Uiso calc . 1 1 C C12 0.4878(3) 0.1255(4) 0.66804(18) 0.0569(13) Uani d . 1 1 H H12A 0.5438 0.1076 0.6608 0.068 Uiso calc . 1 1 H H12B 0.4734 0.1035 0.7007 0.068 Uiso calc . 1 1 C C13 0.4314(2) 0.0870(3) 0.63017(16) 0.0395(10) Uani d D 1 1 H H13 0.409(2) 0.0370(18) 0.6407(15) 0.053(13) Uiso d D 1 1 C C14 0.4256(2) 0.1116(3) 0.58242(16) 0.0385(10) Uani d D 1 1 H H14 0.399(2) 0.076(2) 0.5604(11) 0.035(11) Uiso d D 1 1 C C15 0.4765(3) 0.1803(3) 0.55893(17) 0.0521(12) Uani d . 1 1 H H15A 0.4877 0.1650 0.5246 0.063 Uiso calc . 1 1 H H15B 0.5289 0.1840 0.5762 0.063 Uiso calc . 1 1 C C16 0.4352(3) 0.2658(3) 0.56028(19) 0.0592(13) Uani d . 1 1 H H16A 0.4770 0.3100 0.5589 0.071 Uiso calc . 1 1 H H16B 0.4010 0.2716 0.5308 0.071 Uiso calc . 1 1 C C17 0.2195(2) -0.0158(2) 0.84536(13) 0.0268(8) Uani d . 1 1 C C18 0.1040(3) -0.1135(3) 0.85686(16) 0.0452(11) Uani d . 1 1 H H18A 0.0546 -0.0787 0.8550 0.054 Uiso calc . 1 1 H H18B 0.0936 -0.1604 0.8796 0.054 Uiso calc . 1 1 C C19 0.1239(3) -0.1476(3) 0.80667(17) 0.0488(11) Uani d . 1 1 H H19A 0.1702 -0.1867 0.8089 0.059 Uiso calc . 1 1 H H19B 0.0770 -0.1788 0.7935 0.059 Uiso calc . 1 1 C C20 0.1447(3) -0.0753(3) 0.77315(16) 0.0486(11) Uani d . 1 1 H H20A 0.1654 -0.0972 0.7417 0.058 Uiso calc . 1 1 H H20B 0.0956 -0.0419 0.7664 0.058 Uiso calc . 1 1 C C21 0.2480(2) 0.0378(3) 0.76332(14) 0.0395(10) Uani d . 1 1 H H21A 0.2705 0.0063 0.7353 0.047 Uiso calc . 1 1 H H21B 0.2937 0.0637 0.7810 0.047 Uiso calc . 1 1 C C22 0.1927(2) 0.1073(3) 0.74396(14) 0.0373(9) Uani d . 1 1 H H22A 0.1545 0.1251 0.7697 0.045 Uiso calc . 1 1 H H22B 0.1613 0.0866 0.7157 0.045 Uiso calc . 1 1 C C23 0.2462(2) 0.1819(3) 0.72838(13) 0.0355(9) Uani d . 1 1 H H23A 0.2623 0.2136 0.7579 0.043 Uiso calc . 1 1 H H23B 0.2959 0.1600 0.7130 0.043 Uiso calc . 1 1 C C24 0.1405(3) 0.2910(3) 0.71502(15) 0.0438(10) Uani d . 1 1 H H24A 0.1573 0.3133 0.7472 0.053 Uiso calc . 1 1 H H24B 0.0919 0.2560 0.7198 0.053 Uiso calc . 1 1 C C25 0.1214(3) 0.3630(3) 0.68061(17) 0.0451(11) Uani d . 1 1 H H25A 0.0730 0.3935 0.6923 0.054 Uiso calc . 1 1 H H25B 0.1672 0.4028 0.6797 0.054 Uiso calc . 1 1 C C26 0.1061(3) 0.3280(3) 0.63002(16) 0.0447(11) Uani d . 1 1 H H26A 0.0572 0.2924 0.6305 0.054 Uiso calc . 1 1 H H26B 0.0968 0.3746 0.6068 0.054 Uiso calc . 1 1 C C27 0.2226(2) 0.2346(2) 0.64542(13) 0.0264(8) Uani d . 1 1 C C28 0.1766(2) -0.0514(2) 0.92925(13) 0.0331(9) Uani d . 1 1 H H28 0.2234 -0.0136 0.9360 0.040 Uiso calc . 1 1 C C29 0.1865(2) 0.2654(3) 0.55998(14) 0.0368(9) Uani d . 1 1 H H29 0.2368 0.2317 0.5554 0.044 Uiso calc . 1 1 C C281 0.1927(3) -0.1345(3) 0.95619(17) 0.0528(12) Uani d . 1 1 H H28A 0.2419 -0.1603 0.9433 0.079 Uiso calc . 1 1 H H28B 0.1470 -0.1725 0.9512 0.079 Uiso calc . 1 1 H H28C 0.1993 -0.1235 0.9912 0.079 Uiso calc . 1 1 C C282 0.1006(3) -0.0072(3) 0.94842(16) 0.0490(11) Uani d . 1 1 H H28D 0.0925 0.0452 0.9305 0.073 Uiso calc . 1 1 H H28E 0.1072 0.0051 0.9833 0.073 Uiso calc . 1 1 H H28F 0.0537 -0.0437 0.9438 0.073 Uiso calc . 1 1 C C291 0.1980(3) 0.3475(3) 0.53222(18) 0.0625(14) Uani d . 1 1 H H29A 0.2437 0.3783 0.5462 0.094 Uiso calc . 1 1 H H29B 0.1490 0.3814 0.5349 0.094 Uiso calc . 1 1 H H29C 0.2088 0.3353 0.4978 0.094 Uiso calc . 1 1 C C292 0.1166(3) 0.2136(3) 0.53902(17) 0.0563(13) Uani d . 1 1 H H29D 0.1112 0.1614 0.5576 0.084 Uiso calc . 1 1 H H29E 0.1276 0.2006 0.5047 0.084 Uiso calc . 1 1 H H29F 0.0664 0.2458 0.5414 0.084 Uiso calc . 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.02475(15) 0.02505(17) 0.03142(17) -0.00038(12) -0.00464(12) 0.00325(12) Rh2 0.02445(15) 0.02526(17) 0.02930(16) 0.00086(12) 0.00006(11) 0.00182(12) Br1 0.0385(2) 0.0333(2) 0.0520(3) 0.00655(18) -0.00447(18) -0.00114(19) Br2 0.0444(3) 0.0330(2) 0.0680(3) -0.00669(19) -0.0033(2) -0.0044(2) N1 0.0352(17) 0.0279(17) 0.0307(17) -0.0085(14) -0.0037(13) 0.0025(14) N4 0.0290(16) 0.0339(18) 0.0320(18) 0.0062(14) -0.0016(13) 0.0006(14) N2 0.0377(18) 0.0363(19) 0.0280(18) -0.0069(15) -0.0054(13) 0.0036(14) N3 0.0322(17) 0.0363(19) 0.0272(18) 0.0076(14) 0.0031(13) 0.0045(14) C1 0.036(2) 0.041(3) 0.062(3) 0.011(2) 0.001(2) -0.009(2) C2 0.040(2) 0.031(2) 0.065(3) 0.007(2) -0.017(2) 0.008(2) C3 0.095(4) 0.066(4) 0.077(4) 0.015(3) -0.051(3) 0.008(3) C4 0.104(5) 0.061(4) 0.073(4) -0.003(3) -0.051(3) 0.003(3) C5 0.047(3) 0.038(3) 0.061(3) -0.004(2) -0.025(2) -0.005(2) C6 0.035(2) 0.037(3) 0.081(4) -0.009(2) -0.007(2) 0.008(2) C7 0.047(3) 0.075(4) 0.118(5) -0.017(3) 0.024(3) 0.000(4) C8 0.048(3) 0.090(5) 0.105(5) 0.000(3) 0.026(3) -0.009(4) C9 0.037(2) 0.028(2) 0.061(3) -0.0046(19) 0.007(2) 0.001(2) C10 0.031(2) 0.051(3) 0.054(3) -0.008(2) -0.001(2) -0.017(2) C11 0.035(2) 0.085(4) 0.066(3) -0.003(3) -0.013(2) -0.016(3) C12 0.034(2) 0.084(4) 0.052(3) 0.012(2) -0.005(2) 0.014(3) C13 0.027(2) 0.042(3) 0.049(3) 0.0093(18) 0.0050(18) 0.011(2) C14 0.034(2) 0.038(2) 0.043(3) 0.0072(19) 0.0063(18) -0.004(2) C15 0.048(3) 0.063(3) 0.046(3) 0.002(2) 0.016(2) 0.009(2) C16 0.057(3) 0.052(3) 0.069(3) -0.011(3) 0.022(2) 0.017(3) C17 0.0278(19) 0.0232(19) 0.029(2) 0.0052(16) -0.0032(15) 0.0003(15) C18 0.044(2) 0.042(3) 0.049(3) -0.017(2) -0.002(2) -0.002(2) C19 0.059(3) 0.038(3) 0.050(3) -0.011(2) -0.008(2) -0.008(2) C20 0.060(3) 0.048(3) 0.038(2) -0.010(2) -0.016(2) -0.003(2) C21 0.039(2) 0.051(3) 0.029(2) 0.002(2) 0.0016(17) 0.0095(19) C22 0.034(2) 0.047(3) 0.031(2) -0.0024(18) -0.0012(16) 0.0110(19) C23 0.034(2) 0.045(2) 0.027(2) 0.0012(18) -0.0025(16) 0.0057(18) C24 0.046(2) 0.046(3) 0.040(2) 0.010(2) 0.0085(19) -0.003(2) C25 0.045(2) 0.035(2) 0.054(3) 0.013(2) 0.009(2) -0.003(2) C26 0.039(2) 0.043(3) 0.052(3) 0.017(2) -0.0019(19) 0.002(2) C27 0.0277(18) 0.0199(18) 0.032(2) -0.0014(15) 0.0031(15) 0.0058(15) C28 0.040(2) 0.031(2) 0.028(2) -0.0028(17) 0.0012(16) 0.0057(17) C29 0.040(2) 0.042(2) 0.029(2) 0.0047(19) -0.0057(17) 0.0047(18) C281 0.070(3) 0.044(3) 0.045(3) 0.008(2) 0.005(2) 0.015(2) C282 0.051(3) 0.048(3) 0.048(3) 0.008(2) 0.008(2) 0.003(2) C291 0.095(4) 0.051(3) 0.041(3) 0.004(3) -0.004(2) 0.014(2) C292 0.054(3) 0.064(3) 0.050(3) -0.006(2) -0.017(2) -0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 '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 C17 Rh1 C1 90.89(16) C17 Rh1 C2 91.66(15) C1 Rh1 C2 38.61(18) C17 Rh1 C5 161.56(17) C1 Rh1 C5 94.95(19) C2 Rh1 C5 82.20(17) C17 Rh1 C6 162.59(17) C1 Rh1 C6 80.86(18) C2 Rh1 C6 91.34(18) C5 Rh1 C6 35.71(18) C17 Rh1 Br1 89.38(10) C1 Rh1 Br1 159.60(13) C2 Rh1 Br1 161.76(14) C5 Rh1 Br1 91.15(12) C6 Rh1 Br1 93.08(13) C27 Rh2 C9 90.25(15) C27 Rh2 C10 92.15(16) C9 Rh2 C10 38.84(18) C27 Rh2 C13 158.99(15) C9 Rh2 C13 97.05(16) C10 Rh2 C13 81.59(17) C27 Rh2 C14 164.93(15) C9 Rh2 C14 81.46(16) C10 Rh2 C14 89.25(17) C13 Rh2 C14 35.85(15) C27 Rh2 Br2 89.27(10) C9 Rh2 Br2 158.18(13) C10 Rh2 Br2 162.95(14) C13 Rh2 Br2 91.07(12) C14 Rh2 Br2 93.78(11) C17 N1 C18 122.7(3) C17 N1 C28 120.1(3) C18 N1 C28 116.4(3) C27 N4 C26 122.3(3) C27 N4 C29 119.7(3) C26 N4 C29 117.4(3) C17 N2 C21 119.2(3) C17 N2 C20 124.6(3) C21 N2 C20 115.6(3) C27 N3 C23 119.8(3) C27 N3 C24 124.1(3) C23 N3 C24 115.3(3) C2 C1 C8 125.8(5) C2 C1 Rh1 70.9(2) C8 C1 Rh1 112.6(3) C2 C1 H1 114(3) C8 C1 H1 114(3) Rh1 C1 H1 110(3) C1 C2 C3 123.7(5) C1 C2 Rh1 70.5(2) C3 C2 Rh1 111.2(3) C1 C2 H2 122(3) C3 C2 H2 112(3) Rh1 C2 H2 105(3) C4 C3 C2 117.2(4) C4 C3 H3A 108.0 C2 C3 H3A 108.0 C4 C3 H3B 108.0 C2 C3 H3B 108.0 H3A C3 H3B 107.2 C3 C4 C5 115.6(4) C3 C4 H4A 108.4 C5 C4 H4A 108.4 C3 C4 H4B 108.4 C5 C4 H4B 108.4 H4A C4 H4B 107.4 C6 C5 C4 126.5(5) C6 C5 Rh1 72.5(3) C4 C5 Rh1 107.9(3) C6 C5 H5 119(3) C4 C5 H5 113(3) Rh1 C5 H5 99(3) C5 C6 C7 125.3(5) C5 C6 Rh1 71.8(3) C7 C6 Rh1 110.7(3) C5 C6 H6 114(2) C7 C6 H6 119(2) Rh1 C6 H6 101(2) C8 C7 C6 115.8(4) C8 C7 H7A 108.3 C6 C7 H7A 108.3 C8 C7 H7B 108.3 C6 C7 H7B 108.3 H7A C7 H7B 107.4 C7 C8 C1 115.7(5) C7 C8 H8A 108.4 C1 C8 H8A 108.4 C7 C8 H8B 108.4 C1 C8 H8B 108.4 H8A C8 H8B 107.4 C10 C9 C16 126.3(4) C10 C9 Rh2 71.3(2) C16 C9 Rh2 109.8(3) C10 C9 H9 114(2) C16 C9 H9 114(2) Rh2 C9 H9 111(2) C9 C10 C11 124.2(4) C9 C10 Rh2 69.9(2) C11 C10 Rh2 113.2(3) C9 C10 H10 120(3) C11 C10 H10 112(3) Rh2 C10 H10 106(3) C12 C11 C10 113.9(4) C12 C11 H11A 108.8 C10 C11 H11A 108.8 C12 C11 H11B 108.8 C10 C11 H11B 108.8 H11A C11 H11B 107.7 C13 C12 C11 113.6(4) C13 C12 H12A 108.8 C11 C12 H12A 108.8 C13 C12 H12B 108.8 C11 C12 H12B 108.8 H12A C12 H12B 107.7 C14 C13 C12 125.3(4) C14 C13 Rh2 72.8(2) C12 C13 Rh2 108.6(3) C14 C13 H13 121(3) C12 C13 H13 112(3) Rh2 C13 H13 101(3) C13 C14 C15 124.7(4) C13 C14 Rh2 71.3(2) C15 C14 Rh2 110.7(3) C13 C14 H14 118(2) C15 C14 H14 115(2) Rh2 C14 H14 102(2) C14 C15 C16 112.5(3) C14 C15 H15A 109.1 C16 C15 H15A 109.1 C14 C15 H15B 109.1 C16 C15 H15B 109.1 H15A C15 H15B 107.8 C9 C16 C15 114.0(4) C9 C16 H16A 108.8 C15 C16 H16A 108.8 C9 C16 H16B 108.8 C15 C16 H16B 108.8 H16A C16 H16B 107.7 N1 C17 N2 117.8(3) N1 C17 Rh1 122.6(3) N2 C17 Rh1 119.6(3) N1 C18 C19 110.0(3) N1 C18 H18A 109.7 C19 C18 H18A 109.7 N1 C18 H18B 109.7 C19 C18 H18B 109.7 H18A C18 H18B 108.2 C20 C19 C18 109.0(4) C20 C19 H19A 109.9 C18 C19 H19A 109.9 C20 C19 H19B 109.9 C18 C19 H19B 109.9 H19A C19 H19B 108.3 N2 C20 C19 109.9(3) N2 C20 H20A 109.7 C19 C20 H20A 109.7 N2 C20 H20B 109.7 C19 C20 H20B 109.7 H20A C20 H20B 108.2 N2 C21 C22 113.4(3) N2 C21 H21A 108.9 C22 C21 H21A 108.9 N2 C21 H21B 108.9 C22 C21 H21B 108.9 H21A C21 H21B 107.7 C21 C22 C23 108.1(3) C21 C22 H22A 110.1 C23 C22 H22A 110.1 C21 C22 H22B 110.1 C23 C22 H22B 110.1 H22A C22 H22B 108.4 N3 C23 C22 113.7(3) N3 C23 H23A 108.8 C22 C23 H23A 108.8 N3 C23 H23B 108.8 C22 C23 H23B 108.8 H23A C23 H23B 107.7 N3 C24 C25 109.3(3) N3 C24 H24A 109.8 C25 C24 H24A 109.8 N3 C24 H24B 109.8 C25 C24 H24B 109.8 H24A C24 H24B 108.3 C26 C25 C24 108.9(3) C26 C25 H25A 109.9 C24 C25 H25A 109.9 C26 C25 H25B 109.9 C24 C25 H25B 109.9 H25A C25 H25B 108.3 N4 C26 C25 110.1(3) N4 C26 H26A 109.6 C25 C26 H26A 109.6 N4 C26 H26B 109.6 C25 C26 H26B 109.6 H26A C26 H26B 108.2 N4 C27 N3 118.8(3) N4 C27 Rh2 123.1(3) N3 C27 Rh2 118.0(2) N1 C28 C282 110.4(3) N1 C28 C281 112.6(3) C282 C28 C281 111.9(3) N1 C28 H28 107.2 C282 C28 H28 107.2 C281 C28 H28 107.2 N4 C29 C291 113.0(4) N4 C29 C292 110.6(3) C291 C29 C292 111.8(4) N4 C29 H29 107.0 C291 C29 H29 107.0 C292 C29 H29 107.0 C28 C281 H28A 109.5 C28 C281 H28B 109.5 H28A C281 H28B 109.5 C28 C281 H28C 109.5 H28A C281 H28C 109.5 H28B C281 H28C 109.5 C28 C282 H28D 109.5 C28 C282 H28E 109.5 H28D C282 H28E 109.5 C28 C282 H28F 109.5 H28D C282 H28F 109.5 H28E C282 H28F 109.5 C29 C291 H29A 109.5 C29 C291 H29B 109.5 H29A C291 H29B 109.5 C29 C291 H29C 109.5 H29A C291 H29C 109.5 H29B C291 H29C 109.5 C29 C292 H29D 109.5 C29 C292 H29E 109.5 H29D C292 H29E 109.5 C29 C292 H29F 109.5 H29D C292 H29F 109.5 H29E C292 H29F 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Rh1 C17 2.033(4) Rh1 C1 2.104(4) Rh1 C2 2.108(4) Rh1 C5 2.198(4) Rh1 C6 2.207(4) Rh1 Br1 2.5239(5) Rh2 C27 2.043(3) Rh2 C9 2.103(4) Rh2 C10 2.121(4) Rh2 C13 2.191(4) Rh2 C14 2.210(4) Rh2 Br2 2.5205(5) N1 C17 1.346(5) N1 C18 1.461(5) N1 C28 1.476(5) N4 C27 1.338(5) N4 C26 1.460(5) N4 C29 1.483(5) N2 C17 1.350(5) N2 C21 1.461(5) N2 C20 1.466(5) N3 C27 1.346(5) N3 C23 1.460(5) N3 C24 1.465(5) C1 C2 1.393(7) C1 C8 1.505(7) C1 H1 0.927(19) C2 C3 1.515(6) C2 H2 0.910(19) C3 C4 1.459(8) C3 H3A 0.9800 C3 H3B 0.9800 C4 C5 1.498(7) C4 H4A 0.9800 C4 H4B 0.9800 C5 C6 1.351(7) C5 H5 0.928(19) C6 C7 1.513(7) C6 H6 0.930(18) C7 C8 1.463(8) C7 H7A 0.9800 C7 H7B 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C9 C10 1.405(6) C9 C16 1.504(6) C9 H9 0.941(18) C10 C11 1.519(6) C10 H10 0.932(19) C11 C12 1.513(8) C11 H11A 0.9800 C11 H11B 0.9800 C12 C13 1.510(7) C12 H12A 0.9800 C12 H12B 0.9800 C13 C14 1.355(6) C13 H13 0.918(19) C14 C15 1.510(6) C14 H14 0.935(18) C15 C16 1.512(7) C15 H15A 0.9800 C15 H15B 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C18 C19 1.499(6) C18 H18A 0.9800 C18 H18B 0.9800 C19 C20 1.499(6) C19 H19A 0.9800 C19 H19B 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C21 C22 1.518(5) C21 H21A 0.9800 C21 H21B 0.9800 C22 C23 1.529(6) C22 H22A 0.9800 C22 H22B 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C24 C25 1.504(6) C24 H24A 0.9800 C24 H24B 0.9800 C25 C26 1.500(6) C25 H25A 0.9800 C25 H25B 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C28 C282 1.520(6) C28 C281 1.525(6) C28 H28 0.9900 C29 C291 1.511(6) C29 C292 1.519(6) C29 H29 0.9900 C281 H28A 0.9700 C281 H28B 0.9700 C281 H28C 0.9700 C282 H28D 0.9700 C282 H28E 0.9700 C282 H28F 0.9700 C291 H29A 0.9700 C291 H29B 0.9700 C291 H29C 0.9700 C292 H29D 0.9700 C292 H29E 0.9700 C292 H29F 0.9700