#------------------------------------------------------------------------------ #$Date: 2021-05-20 04:59:10 +0300 (Thu, 20 May 2021) $ #$Revision: 265353 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/74/7707446.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_7707446 loop_ _publ_author_name 'Szczepkowska, Anna M.' 'Janeta, Mateusz' 'Siczek, Mi\/losz' 'Tylus, W\/lodzimierz' 'Trzeciak, Anna M.' 'Bury, Wojciech' _publ_section_title ; Immobilization of Rh(i) precursor in a porphyrin metal--organic framework -- turning on the catalytic activity ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00518A _journal_year 2021 _chemical_formula_moiety 'C56 H36 N4 O12 Rh2, 0.3(C H Cl3)' _chemical_formula_sum 'C56.3 H36.3 Cl0.9 N4 O12 Rh2' _chemical_formula_weight 1198.52 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2021-04-13 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.88(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.301(2) _cell_length_b 29.369(6) _cell_length_c 10.680(2) _cell_measurement_reflns_used 1628 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 21.40 _cell_measurement_theta_min 3.24 _cell_volume 3122.7(11) _computing_cell_refinement 'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlis CCD 1.171.13(Oxford Diffraction ,2003)' _computing_data_reduction 'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)' _computing_molecular_graphics 'Diamond, Crystal Impact' _computing_publication_material 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'KUMA KM4 with Sapphire CCD detector' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2437 _diffrn_reflns_av_unetI/netI 0.2932 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.930 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 20754 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.930 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.906 _diffrn_reflns_theta_min 2.774 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.275 _exptl_crystal_description needle _exptl_crystal_F_000 1207 _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _refine_diff_density_max 2.468 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.214 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 351 _refine_ls_number_reflns 6938 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.2728 _refine_ls_R_factor_gt 0.1312 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1790P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3121 _refine_ls_wR_factor_ref 0.4174 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2486 _reflns_number_total 6938 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00518a2.cif _cod_data_source_block aww516a _cod_original_cell_volume 3122.7(12) _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C56.30 H36.30 Cl0.90 N4 O12 Rh2' _cod_database_code 7707446 _shelx_shelxl_version_number 2018/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL AWW516 in P21/c #14 aww516a.res created by SHELXL-2018/1 at 11:31:17 on 25-Nov-2020 REM reset to P21/c #14 CELL 0.71073 10.301281 29.368791 10.679659 90 104.8761 90 ZERR 2 0.002487 0.005858 0.002019 0 0.0228 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Rh UNIT 112.6 72.6 1.8 8 24 4 DFIX 2.8 0.01 Cl1 Cl2 Cl1 Cl3 Cl2 Cl3 DFIX 2.8 0.01 Cl4 Cl5 Cl4 Cl6 Cl5 Cl6 DFIX 2.8 0.01 Cl7 Cl8 Cl7 Cl9 Cl8 Cl9 DFIX 1.7 0.01 C3R Cl7 C3R Cl8 C3R Cl9 DFIX 1.7 0.01 C1R Cl1 C1R Cl2 C1R Cl3 DFIX 1.7 0.01 C2R Cl4 C2R Cl5 C2R Cl6 EADP C11 O11 C12 O12 C10 C9 EADP Cl4 C1R C2R C3R L.S. 20 PLAN 20 TEMP -173 CONN 4 Cl5 BOND fmap 2 acta REM REM REM WGHT 0.179000 FVAR 0.29227 RH 6 1.112805 0.502627 0.624351 11.00000 0.03995 0.03682 = 0.02329 -0.00006 0.00181 -0.00100 C11 1 1.059256 0.532808 0.756090 11.00000 0.03993 0.05576 = 0.02624 -0.00996 -0.00029 -0.01524 O11 5 1.031624 0.550965 0.838865 11.00000 0.03993 0.05576 = 0.02624 -0.00996 -0.00029 -0.01524 C12 1 1.234855 0.550167 0.620208 11.00000 0.03993 0.05576 = 0.02624 -0.00996 -0.00029 -0.01524 O12 5 1.310514 0.576514 0.627398 11.00000 0.03993 0.05576 = 0.02624 -0.00996 -0.00029 -0.01524 N1 4 1.177829 0.465243 0.486300 11.00000 0.03080 0.03016 = 0.01290 -0.00148 0.00201 -0.00491 N2 4 0.994580 0.446981 0.635705 11.00000 0.05378 0.03413 = 0.02525 0.01425 0.01711 0.01906 C1 1 1.239548 0.481033 0.389406 11.00000 0.02905 0.04909 = 0.02351 -0.01019 0.00876 -0.00375 C2 1 1.317932 0.443532 0.356169 11.00000 0.02526 0.03604 = 0.04616 -0.00535 0.01291 0.00161 AFIX 43 H2 2 1.372629 0.444299 0.296855 11.00000 -1.20000 AFIX 0 C3 1 1.296758 0.407921 0.426485 11.00000 0.06429 0.03924 = 0.02745 0.00511 0.01873 0.00872 AFIX 43 H3 2 1.334620 0.378499 0.424865 11.00000 -1.20000 AFIX 0 C4 1 1.208051 0.420788 0.505022 11.00000 0.04433 0.03740 = 0.01747 -0.00086 0.01038 -0.00819 C5 1 1.156688 0.393644 0.584947 11.00000 0.04428 0.02821 = 0.02270 0.00837 -0.00427 -0.00419 C6 1 1.048004 0.403437 0.636530 11.00000 0.03788 0.04293 = 0.01442 0.00187 -0.00504 -0.01633 C7 1 0.965829 0.372278 0.687606 11.00000 0.04926 0.03559 = 0.04157 -0.00376 0.01267 0.00997 AFIX 43 H7 2 0.981797 0.340660 0.703013 11.00000 -1.20000 AFIX 0 C8 1 0.861345 0.396580 0.709568 11.00000 0.06240 0.02385 = 0.04877 -0.00413 0.00274 0.00527 AFIX 43 H8 2 0.790483 0.385047 0.742448 11.00000 -1.20000 AFIX 0 C9 1 0.877806 0.441743 0.674655 11.00000 0.03993 0.05576 = 0.02624 -0.00996 -0.00029 -0.01524 C10 1 0.777621 0.475906 0.674169 11.00000 0.03993 0.05576 = 0.02624 -0.00996 -0.00029 -0.01524 O51 5 1.461130 0.203727 0.762852 11.00000 0.08206 0.03665 = 0.06585 0.00003 0.00598 0.01051 O52 5 1.357360 0.183118 0.555790 11.00000 0.12484 0.04486 = 0.05214 -0.01527 0.01333 0.03018 C51 1 1.210565 0.344431 0.603343 11.00000 0.02856 0.04364 = 0.04946 -0.00153 0.00949 -0.00423 C52 1 1.180745 0.314322 0.501919 11.00000 0.07120 0.05878 = 0.03196 0.00061 -0.00640 0.00322 AFIX 43 H52 2 1.121240 0.323165 0.422034 11.00000 -1.20000 AFIX 0 C53 1 1.236409 0.271242 0.514780 11.00000 0.08702 0.03972 = 0.04600 -0.01125 0.00181 0.03667 AFIX 43 H53 2 1.217492 0.250999 0.442992 11.00000 -1.20000 AFIX 0 C54 1 1.318436 0.257719 0.630289 11.00000 0.03984 0.03114 = 0.05990 0.00323 0.01817 0.00209 C55 1 1.340938 0.287878 0.737754 11.00000 0.08092 0.03489 = 0.02225 0.00118 0.00545 0.01729 AFIX 43 H55 2 1.390239 0.278068 0.821185 11.00000 -1.20000 AFIX 0 C56 1 1.292158 0.330038 0.720218 11.00000 0.09239 0.02398 = 0.03200 -0.00658 -0.02046 -0.00279 AFIX 43 H56 2 1.314245 0.350902 0.790473 11.00000 -1.20000 AFIX 0 C57 1 1.379700 0.211763 0.641863 11.00000 0.06015 0.04996 = 0.05708 0.00490 0.02128 0.01003 C58 1 1.532378 0.160912 0.784409 11.00000 0.10714 0.04830 = 0.07714 0.00441 0.01044 0.03611 AFIX 137 H58A 2 1.566749 0.155734 0.877721 11.00000 -1.50000 H58B 2 1.607565 0.161800 0.743854 11.00000 -1.50000 H58C 2 1.471164 0.136152 0.746280 11.00000 -1.50000 AFIX 0 O101 5 0.285031 0.432585 0.922158 11.00000 0.02938 0.06015 = 0.03595 0.00406 0.00829 -0.00921 O102 5 0.450157 0.434532 1.111155 11.00000 0.04312 0.04926 = 0.02564 -0.00547 0.01325 -0.00376 C101 1 0.682010 0.465368 0.754967 11.00000 0.03033 0.04892 = 0.01857 0.00596 0.00489 -0.00209 C102 1 0.736615 0.456689 0.884742 11.00000 0.02557 0.05679 = 0.05102 0.00188 0.00994 0.00064 AFIX 43 H102 2 0.830993 0.456565 0.921216 11.00000 -1.20000 AFIX 0 C103 1 0.645244 0.447948 0.961293 11.00000 0.04929 0.03471 = 0.02882 -0.01056 0.00240 -0.00051 AFIX 43 H103 2 0.679632 0.443234 1.051766 11.00000 -1.20000 AFIX 0 C104 1 0.506562 0.446043 0.908172 11.00000 0.03286 0.03571 = 0.01694 0.00368 -0.00219 -0.01450 C105 1 0.458812 0.454456 0.777156 11.00000 0.02859 0.04894 = 0.03545 0.00575 0.00634 0.00022 AFIX 43 H105 2 0.365104 0.452853 0.737768 11.00000 -1.20000 AFIX 0 C106 1 0.547261 0.465287 0.702345 11.00000 0.03795 0.05241 = 0.01496 0.00166 -0.00929 -0.00299 AFIX 43 H106 2 0.512782 0.472704 0.613411 11.00000 -1.20000 AFIX 0 C107 1 0.412269 0.436685 0.995338 11.00000 0.04816 0.02723 = 0.04961 0.01272 0.03117 0.00126 C108 1 0.193168 0.424671 0.997418 11.00000 0.05184 0.07648 = 0.04704 -0.00040 0.01694 0.00234 AFIX 137 H10A 2 0.197691 0.449805 1.058752 11.00000 -1.50000 H10B 2 0.215879 0.396061 1.045255 11.00000 -1.50000 H10C 2 0.102054 0.422646 0.940582 11.00000 -1.50000 AFIX 0 PART 1 C1R 1 0.918123 0.205628 0.578827 10.05000 0.01812 AFIX 13 H1R 2 0.928261 0.224490 0.503956 10.05000 -1.20000 AFIX 0 CL1 3 0.904965 0.241501 0.699714 10.05000 0.05091 CL2 3 0.777007 0.173590 0.528296 10.05000 0.02434 CL3 3 1.056386 0.172038 0.626443 10.05000 0.04770 PART 0 PART 2 C2R 1 0.780818 0.245241 0.589281 10.05000 0.01812 AFIX 13 H2R 2 0.793687 0.267344 0.522259 10.05000 -1.20000 AFIX 0 CL4 3 0.725755 0.274617 0.702639 10.05000 0.01812 CL5 3 0.665465 0.205940 0.514699 10.05000 0.07522 CL6 3 0.931247 0.220068 0.656479 10.05000 0.08824 PART 0 PART 3 C3R 1 0.842997 0.242887 0.621388 10.05000 0.01812 AFIX 13 H3R 2 0.892453 0.269234 0.596318 10.05000 -1.20000 AFIX 0 CL7 3 0.917588 0.194236 0.589062 10.05000 0.05569 CL8 3 0.852931 0.247357 0.782229 10.05000 0.15109 CL9 3 0.680717 0.245725 0.532510 10.05000 0.03629 HKLF 4 REM AWW516 in P21/c #14 REM R1 = 0.1312 for 2486 Fo > 4sig(Fo) and 0.2728 for all 6938 data REM 351 parameters refined using 18 restraints END WGHT 0.1791 0.0000 REM Highest difference peak 2.468, deepest hole -1.627, 1-sigma level 0.214 Q1 1 0.6626 0.5001 1.1251 11.00000 0.05 1.98 Q2 1 0.9869 0.5011 0.5989 11.00000 0.05 1.91 Q3 1 1.2348 0.5033 0.6554 11.00000 0.05 1.47 Q4 1 1.1191 0.5348 0.6318 11.00000 0.05 1.40 Q5 1 1.1270 0.4648 0.6326 11.00000 0.05 1.38 Q6 1 0.7269 0.2607 0.5976 11.00000 0.05 0.97 Q7 1 0.8991 0.2404 0.5892 11.00000 0.05 0.84 Q8 1 0.8454 0.1679 0.5542 11.00000 0.05 0.81 Q9 1 0.7227 0.2347 0.4991 11.00000 0.05 0.79 Q10 1 0.9556 0.1773 0.5815 11.00000 0.05 0.78 Q11 1 1.1774 0.4934 0.4749 11.00000 0.05 0.77 Q12 1 1.0000 0.5000 0.5000 10.50000 0.05 0.76 Q13 1 0.6711 0.1812 0.5157 11.00000 0.05 0.75 Q14 1 1.2126 0.4780 0.3390 11.00000 0.05 0.75 Q15 1 0.6798 0.4638 0.9942 11.00000 0.05 0.69 Q16 1 0.6304 0.2347 0.5255 11.00000 0.05 0.69 Q17 1 0.9903 0.1879 0.6166 11.00000 0.05 0.66 Q18 1 0.7204 0.4518 0.9025 11.00000 0.05 0.66 Q19 1 0.4506 0.4633 0.7591 11.00000 0.05 0.64 Q20 1 1.1231 0.5015 0.3574 11.00000 0.05 0.64 ; _shelx_res_checksum 14795 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 1.11281(11) 0.50263(4) 0.62435(10) 0.0345(4) Uani 1 1 d . . . . . C11 C 1.0593(14) 0.5328(5) 0.7561(14) 0.0422(13) Uani 1 1 d . . . . . O11 O 1.0316(9) 0.5510(3) 0.8389(9) 0.0422(13) Uani 1 1 d . . . . . C12 C 1.2349(15) 0.5502(5) 0.6202(14) 0.0422(13) Uani 1 1 d . . . . . O12 O 1.3105(10) 0.5765(3) 0.6274(9) 0.0422(13) Uani 1 1 d . . . . . N1 N 1.1778(10) 0.4652(3) 0.4863(9) 0.025(2) Uani 1 1 d . . . . . N2 N 0.9946(12) 0.4470(3) 0.6357(11) 0.036(3) Uani 1 1 d . . . . . C1 C 1.2395(13) 0.4810(5) 0.3894(13) 0.034(3) Uani 1 1 d . . . . . C2 C 1.3179(13) 0.4435(4) 0.3562(14) 0.035(3) Uani 1 1 d . . . . . H2 H 1.372629 0.444299 0.296855 0.042 Uiso 1 1 calc R U . . . C3 C 1.2968(16) 0.4079(5) 0.4265(13) 0.042(4) Uani 1 1 d . . . . . H3 H 1.334620 0.378499 0.424865 0.051 Uiso 1 1 calc R U . . . C4 C 1.2081(14) 0.4208(4) 0.5050(12) 0.033(3) Uani 1 1 d . . . . . C5 C 1.1567(14) 0.3936(4) 0.5849(13) 0.034(3) Uani 1 1 d . . . . . C6 C 1.0480(14) 0.4034(4) 0.6365(12) 0.034(3) Uani 1 1 d . . . . . C7 C 0.9658(15) 0.3723(5) 0.6876(14) 0.042(4) Uani 1 1 d . . . . . H7 H 0.981797 0.340660 0.703013 0.050 Uiso 1 1 calc R U . . . C8 C 0.8613(16) 0.3966(4) 0.7096(15) 0.047(4) Uani 1 1 d . . . . . H8 H 0.790483 0.385047 0.742448 0.057 Uiso 1 1 calc R U . . . C9 C 0.8778(15) 0.4417(5) 0.6747(14) 0.0422(13) Uani 1 1 d . . . . . C10 C 0.7776(15) 0.4759(5) 0.6742(14) 0.0422(13) Uani 1 1 d . . . . . O51 O 1.4611(12) 0.2037(3) 0.7629(12) 0.064(3) Uani 1 1 d . . . . . O52 O 1.3574(14) 0.1831(4) 0.5558(12) 0.076(4) Uani 1 1 d . . . . . C51 C 1.2106(14) 0.3444(5) 0.6033(15) 0.041(4) Uani 1 1 d . . . . . C52 C 1.1807(17) 0.3143(6) 0.5019(15) 0.058(5) Uani 1 1 d . . . . . H52 H 1.121240 0.323165 0.422034 0.069 Uiso 1 1 calc R U . . . C53 C 1.2364(18) 0.2712(5) 0.5148(16) 0.060(5) Uani 1 1 d . . . . . H53 H 1.217492 0.250999 0.442992 0.072 Uiso 1 1 calc R U . . . C54 C 1.3184(15) 0.2577(4) 0.6303(16) 0.043(4) Uani 1 1 d . . . . . C55 C 1.3409(16) 0.2879(4) 0.7378(14) 0.047(4) Uani 1 1 d . . . . . H55 H 1.390239 0.278068 0.821185 0.057 Uiso 1 1 calc R U . . . C56 C 1.2922(18) 0.3300(4) 0.7202(15) 0.056(5) Uani 1 1 d . . . . . H56 H 1.314245 0.350902 0.790473 0.067 Uiso 1 1 calc R U . . . C57 C 1.3797(18) 0.2118(5) 0.6419(18) 0.055(4) Uani 1 1 d . . . . . C58 C 1.532(2) 0.1609(6) 0.784(2) 0.080(6) Uani 1 1 d . . . . . H58A H 1.566749 0.155734 0.877721 0.120 Uiso 1 1 calc R U . . . H58B H 1.607565 0.161800 0.743854 0.120 Uiso 1 1 calc R U . . . H58C H 1.471164 0.136152 0.746280 0.120 Uiso 1 1 calc R U . . . O101 O 0.2850(10) 0.4326(3) 0.9222(10) 0.042(2) Uani 1 1 d . . . . . O102 O 0.4502(10) 0.4345(3) 1.1112(9) 0.039(2) Uani 1 1 d . . . . . C101 C 0.6820(13) 0.4654(5) 0.7550(12) 0.033(3) Uani 1 1 d . . . . . C102 C 0.7366(15) 0.4567(5) 0.8847(16) 0.044(4) Uani 1 1 d . . . . . H102 H 0.830993 0.456565 0.921216 0.053 Uiso 1 1 calc R U . . . C103 C 0.6452(15) 0.4479(4) 0.9613(14) 0.039(4) Uani 1 1 d . . . . . H103 H 0.679632 0.443234 1.051766 0.047 Uiso 1 1 calc R U . . . C104 C 0.5066(13) 0.4460(4) 0.9082(12) 0.030(3) Uani 1 1 d . . . . . C105 C 0.4588(14) 0.4545(5) 0.7772(14) 0.038(3) Uani 1 1 d . . . . . H105 H 0.365104 0.452853 0.737768 0.046 Uiso 1 1 calc R U . . . C106 C 0.5473(14) 0.4653(5) 0.7023(13) 0.038(3) Uani 1 1 d . . . . . H106 H 0.512782 0.472704 0.613411 0.046 Uiso 1 1 calc R U . . . C107 C 0.4123(16) 0.4367(4) 0.9953(15) 0.038(4) Uani 1 1 d . . . . . C108 C 0.1932(16) 0.4247(6) 0.9974(16) 0.058(5) Uani 1 1 d . . . . . H10A H 0.197691 0.449805 1.058752 0.087 Uiso 1 1 calc R U . . . H10B H 0.215879 0.396061 1.045255 0.087 Uiso 1 1 calc R U . . . H10C H 0.102054 0.422646 0.940582 0.087 Uiso 1 1 calc R U . . . C1R C 0.918(4) 0.2056(14) 0.579(5) 0.018(11) Uiso 0.05 1 d D . P A 1 H1R H 0.928261 0.224490 0.503956 0.022 Uiso 0.05 1 calc R U P A 1 Cl1 Cl 0.905(6) 0.2415(19) 0.700(7) 0.05(2) Uiso 0.05 1 d D . P A 1 Cl2 Cl 0.777(4) 0.1736(17) 0.528(5) 0.024(12) Uiso 0.05 1 d D . P A 1 Cl3 Cl 1.056(4) 0.172(2) 0.626(7) 0.048(19) Uiso 0.05 1 d D . P A 1 C2R C 0.781(6) 0.2452(18) 0.589(5) 0.018(11) Uiso 0.05 1 d D . P B 2 H2R H 0.793687 0.267344 0.522259 0.022 Uiso 0.05 1 calc R U P B 2 Cl4 Cl 0.726(5) 0.2746(15) 0.703(5) 0.018(11) Uiso 0.05 1 d D . P B 2 Cl5 Cl 0.665(7) 0.206(2) 0.515(7) 0.08(3) Uiso 0.05 1 d D . P B 2 Cl6 Cl 0.931(6) 0.220(3) 0.656(10) 0.09(3) Uiso 0.05 1 d D . P B 2 C3R C 0.843(6) 0.2429(19) 0.621(6) 0.018(11) Uiso 0.05 1 d D . P C 3 H3R H 0.892453 0.269234 0.596318 0.022 Uiso 0.05 1 calc R U P C 3 Cl7 Cl 0.918(6) 0.194(2) 0.589(8) 0.06(2) Uiso 0.05 1 d D . P C 3 Cl8 Cl 0.853(11) 0.247(4) 0.782(6) 0.15(6) Uiso 0.05 1 d D . P C 3 Cl9 Cl 0.681(5) 0.246(2) 0.533(6) 0.036(16) Uiso 0.05 1 d D . P C 3 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 Rh 0.0399(7) 0.0368(7) 0.0233(6) -0.0001(5) 0.0018(5) -0.0010(5) C11 0.040(3) 0.056(3) 0.026(3) -0.010(2) 0.000(2) -0.015(2) O11 0.040(3) 0.056(3) 0.026(3) -0.010(2) 0.000(2) -0.015(2) C12 0.040(3) 0.056(3) 0.026(3) -0.010(2) 0.000(2) -0.015(2) O12 0.040(3) 0.056(3) 0.026(3) -0.010(2) 0.000(2) -0.015(2) N1 0.031(6) 0.030(6) 0.013(5) -0.001(4) 0.002(5) -0.005(5) N2 0.054(8) 0.034(6) 0.025(6) 0.014(5) 0.017(6) 0.019(5) C1 0.029(8) 0.049(8) 0.024(7) -0.010(6) 0.009(6) -0.004(6) C2 0.025(8) 0.036(8) 0.046(9) -0.005(7) 0.013(7) 0.002(6) C3 0.064(11) 0.039(8) 0.027(8) 0.005(6) 0.019(8) 0.009(7) C4 0.044(9) 0.037(8) 0.017(7) -0.001(5) 0.010(6) -0.008(6) C5 0.044(9) 0.028(7) 0.023(7) 0.008(5) -0.004(7) -0.004(6) C6 0.038(9) 0.043(8) 0.014(7) 0.002(5) -0.005(6) -0.016(7) C7 0.049(10) 0.036(8) 0.042(9) -0.004(7) 0.013(8) 0.010(7) C8 0.062(11) 0.024(7) 0.049(10) -0.004(6) 0.003(8) 0.005(7) C9 0.040(3) 0.056(3) 0.026(3) -0.010(2) 0.000(2) -0.015(2) C10 0.040(3) 0.056(3) 0.026(3) -0.010(2) 0.000(2) -0.015(2) O51 0.082(9) 0.037(6) 0.066(9) 0.000(5) 0.006(7) 0.011(6) O52 0.125(12) 0.045(7) 0.052(8) -0.015(6) 0.013(8) 0.030(7) C51 0.029(8) 0.044(8) 0.049(10) -0.002(7) 0.009(7) -0.004(6) C52 0.071(13) 0.059(10) 0.032(9) 0.001(8) -0.006(9) 0.003(9) C53 0.087(14) 0.040(9) 0.046(10) -0.011(7) 0.002(10) 0.037(9) C54 0.040(9) 0.031(7) 0.060(11) 0.003(7) 0.018(8) 0.002(6) C55 0.081(12) 0.035(8) 0.022(8) 0.001(6) 0.005(8) 0.017(8) C56 0.092(14) 0.024(7) 0.032(9) -0.007(6) -0.020(9) -0.003(8) C57 0.060(12) 0.050(10) 0.057(12) 0.005(8) 0.021(10) 0.010(8) C58 0.107(17) 0.048(11) 0.077(14) 0.004(10) 0.010(13) 0.036(11) O101 0.029(6) 0.060(6) 0.036(6) 0.004(5) 0.008(5) -0.009(5) O102 0.043(6) 0.049(6) 0.026(6) -0.005(4) 0.013(5) -0.004(5) C101 0.030(8) 0.049(8) 0.019(7) 0.006(6) 0.005(6) -0.002(6) C102 0.026(8) 0.057(9) 0.051(10) 0.002(8) 0.010(7) 0.001(7) C103 0.049(9) 0.035(8) 0.029(8) -0.011(6) 0.002(7) -0.001(7) C104 0.033(8) 0.036(7) 0.017(7) 0.004(5) -0.002(6) -0.014(6) C105 0.029(8) 0.049(8) 0.035(8) 0.006(7) 0.006(7) 0.000(6) C106 0.038(9) 0.052(9) 0.015(7) 0.002(6) -0.009(6) -0.003(7) C107 0.048(10) 0.027(7) 0.050(10) 0.013(6) 0.031(8) 0.001(6) C108 0.052(11) 0.076(12) 0.047(11) 0.000(9) 0.017(9) 0.002(9) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh C12 89.7(6) . . ? C11 Rh N2 92.2(5) . . ? C12 Rh N2 174.8(6) . . ? C11 Rh N1 176.0(5) . . ? C12 Rh N1 92.1(5) . . ? N2 Rh N1 85.7(4) . . ? C11 Rh Rh 112.0(4) . 3_766 ? C12 Rh Rh 112.3(4) . 3_766 ? N2 Rh Rh 71.4(3) . 3_766 ? N1 Rh Rh 70.6(3) . 3_766 ? O11 C11 Rh 177.4(13) . . ? O12 C12 Rh 174.3(13) . . ? C4 N1 C1 107.1(10) . . ? C4 N1 Rh 120.7(8) . . ? C1 N1 Rh 128.9(8) . . ? C9 N2 C6 105.7(11) . . ? C9 N2 Rh 132.9(9) . . ? C6 N2 Rh 119.4(9) . . ? N1 C1 C10 127.7(12) . 3_766 ? N1 C1 C2 108.0(12) . . ? C10 C1 C2 124.2(13) 3_766 . ? C3 C2 C1 105.8(13) . . ? C2 C3 C4 109.9(13) . . ? N1 C4 C5 123.1(13) . . ? N1 C4 C3 109.0(11) . . ? C5 C4 C3 127.9(13) . . ? C4 C5 C6 127.0(12) . . ? C4 C5 C51 116.2(13) . . ? C6 C5 C51 116.1(12) . . ? N2 C6 C5 122.8(11) . . ? N2 C6 C7 108.4(13) . . ? C5 C6 C7 128.6(13) . . ? C8 C7 C6 107.4(13) . . ? C7 C8 C9 107.2(15) . . ? N2 C9 C8 111.2(14) . . ? N2 C9 C10 127.0(13) . . ? C8 C9 C10 121.7(14) . . ? C1 C10 C9 128.5(14) 3_766 . ? C1 C10 C101 116.0(13) 3_766 . ? C9 C10 C101 115.5(13) . . ? C57 O51 C58 117.6(13) . . ? C52 C51 C56 118.6(13) . . ? C52 C51 C5 120.2(14) . . ? C56 C51 C5 121.2(13) . . ? C51 C52 C53 120.6(15) . . ? C54 C53 C52 120.1(14) . . ? C53 C54 C55 118.9(13) . . ? C53 C54 C57 119.5(14) . . ? C55 C54 C57 121.5(15) . . ? C56 C55 C54 119.3(14) . . ? C55 C56 C51 122.2(13) . . ? O52 C57 O51 122.8(14) . . ? O52 C57 C54 124.7(16) . . ? O51 C57 C54 112.4(14) . . ? C107 O101 C108 112.3(12) . . ? C106 C101 C102 121.7(13) . . ? C106 C101 C10 121.0(12) . . ? C102 C101 C10 117.3(13) . . ? C101 C102 C103 116.9(14) . . ? C104 C103 C102 122.3(13) . . ? C105 C104 C103 117.7(13) . . ? C105 C104 C107 122.1(13) . . ? C103 C104 C107 120.1(12) . . ? C104 C105 C106 120.4(13) . . ? C101 C106 C105 120.8(12) . . ? O102 C107 O101 127.1(14) . . ? O102 C107 C104 123.1(14) . . ? O101 C107 C104 109.7(12) . . ? Cl2 C1R Cl3 110.9(9) . . ? Cl2 C1R Cl1 110.9(9) . . ? Cl3 C1R Cl1 110.9(9) . . ? Cl6 C2R Cl5 110.7(9) . . ? Cl6 C2R Cl4 110.8(9) . . ? Cl5 C2R Cl4 110.9(9) . . ? Cl9 C3R Cl8 110.9(9) . . ? Cl9 C3R Cl7 111.0(9) . . ? Cl8 C3R Cl7 110.9(9) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C11 1.862(15) . ? Rh C12 1.887(15) . ? Rh N2 2.060(12) . ? Rh N1 2.082(10) . ? Rh Rh 3.051(2) 3_766 ? C11 O11 1.130(16) . ? C12 O12 1.087(15) . ? N1 C4 1.345(16) . ? N1 C1 1.424(16) . ? N2 C9 1.379(19) . ? N2 C6 1.391(16) . ? C1 C10 1.42(2) 3_766 ? C1 C2 1.462(18) . ? C2 C3 1.338(18) . ? C3 C4 1.440(19) . ? C4 C5 1.370(18) . ? C5 C6 1.40(2) . ? C5 C51 1.543(18) . ? C6 C7 1.445(19) . ? C7 C8 1.361(19) . ? C8 C9 1.400(19) . ? C9 C10 1.44(2) . ? C10 C101 1.499(19) . ? O51 C57 1.37(2) . ? O51 C58 1.444(17) . ? O52 C57 1.224(18) . ? C51 C52 1.37(2) . ? C51 C56 1.38(2) . ? C52 C53 1.38(2) . ? C53 C54 1.36(2) . ? C54 C55 1.421(19) . ? C54 C57 1.482(19) . ? C55 C56 1.331(18) . ? O101 C107 1.348(17) . ? O101 C108 1.409(17) . ? O102 C107 1.199(17) . ? C101 C106 1.357(17) . ? C101 C102 1.38(2) . ? C102 C103 1.42(2) . ? C103 C104 1.396(18) . ? C104 C105 1.381(19) . ? C104 C107 1.533(19) . ? C105 C106 1.394(19) . ? C1R Cl2 1.699(10) . ? C1R Cl3 1.700(10) . ? C1R Cl1 1.699(10) . ? C2R Cl6 1.701(10) . ? C2R Cl5 1.701(10) . ? C2R Cl4 1.698(10) . ? C3R Cl9 1.699(10) . ? C3R Cl8 1.699(10) . ? C3R Cl7 1.699(10) . ?