#------------------------------------------------------------------------------ #$Date: 2021-06-25 04:34:22 +0300 (Fri, 25 Jun 2021) $ #$Revision: 266669 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/77/7707720.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_7707720 loop_ _publ_author_name 'Hill, Anthony' 'Barnett, Harrison J.' _publ_section_title ; Benzyne addition to a metal-carbon multiple bond ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01402A _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C60 H50.5 Cl3.5 P4 Rh2' _chemical_formula_sum 'C60 H50.5 Cl3.5 P4 Rh2' _chemical_formula_weight 1225.28 _space_group_crystal_system tetragonal _space_group_IT_number 92 _space_group_name_Hall 'P 4abw 2nw' _space_group_name_H-M_alt 'P 41 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-10-22 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-03-10 deposited with the CCDC. 2021-06-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.99510(10) _cell_length_b 14.99510(10) _cell_length_c 26.1521(4) _cell_measurement_reflns_used 6864 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 70.7770 _cell_measurement_theta_min 4.1720 _cell_volume 5880.38(11) _computing_cell_refinement 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.1297 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -52.00 22.00 1.00 1.00 -- -36.03 19.00 90.00 74 2 \w 40.00 78.00 1.00 1.00 -- 36.03-125.00 60.00 38 3 \w 56.00 90.00 1.00 1.00 -- 105.15 -95.00 -30.00 34 4 \w 108.00 173.00 1.00 1.00 -- 105.15 111.00 60.00 65 5 \w 104.00 174.00 1.00 1.00 -- 105.15 111.00 -30.00 70 6 \w 106.00 175.00 1.00 1.00 -- 105.15 111.00 0.00 69 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0143410000 _diffrn_orient_matrix_UB_12 0.0228663000 _diffrn_orient_matrix_UB_13 -0.0567924000 _diffrn_orient_matrix_UB_21 -0.0784477000 _diffrn_orient_matrix_UB_22 0.0661886000 _diffrn_orient_matrix_UB_23 0.0023963000 _diffrn_orient_matrix_UB_31 0.0648157000 _diffrn_orient_matrix_UB_32 0.0751768000 _diffrn_orient_matrix_UB_33 0.0154066000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10253 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.952 _diffrn_reflns_theta_min 4.169 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.305 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.384 _exptl_crystal_description plate _exptl_crystal_F_000 2480 _exptl_crystal_size_max 0.243 _exptl_crystal_size_mid 0.222 _exptl_crystal_size_min 0.155 _refine_diff_density_max 0.927 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.095 _refine_ls_abs_structure_details ; Flack x determined using 2173 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.029(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 365 _refine_ls_number_reflns 5538 _refine_ls_number_restraints 97 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0340 _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^)+(0.0602P)^2^+2.7805P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.0999 _reflns_Friedel_coverage 0.719 _reflns_Friedel_fraction_full 0.992 _reflns_Friedel_fraction_max 0.967 _reflns_number_gt 5367 _reflns_number_total 5538 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01402a2.cif _cod_data_source_block hb_1285_9_1_scale _cod_original_cell_volume 5880.38(12) _cod_original_formula_sum 'C60 H50.50 Cl3.50 P4 Rh2' _cod_database_code 7707720 _shelx_shelxl_version_number 2016/6 _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. ; _reflns_odcompleteness_completeness 99.54 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Rigid bond restraints C7, C5, C3, C6, C4, C2 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 C10, C8, C12, C13, C11, C9 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 Rh1, C8 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 3. Uiso/Uaniso restraints and constraints C7 \\sim C5 \\sim C3 \\sim C6 \\sim C4 \\sim C2: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 C10 \\sim C8 \\sim C12 \\sim C13 \\sim C11 \\sim C9: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: Cl3(0.25) C7(0.5) H7(0.5) C6(0.5) H6(0.5) C5(0.5) H5(0.5) C4(0.5) H4(0.5) C3(0.5) C2(0.5) C8(0.25) C13(0.25) H13(0.25) C12(0.25) H12(0.25) C11(0.25) H11(0.25) C10(0.25) H10(0.25) C9(0.25) H9(0.25) 5.a Secondary CH2 refined with riding coordinates: C14(H14A,H14B) 5.b Aromatic/amide H refined with riding coordinates: C7(H7), C6(H6), C5(H5), C4(H4), C44(H44), C53(H53), C54(H54), C36(H36), C13(H13), C12(H12), C11(H11), C10(H10), C9(H9), C46(H46), C32(H32), C43(H43), C22(H22), C56(H56), C45(H45), C23(H23), C42(H42), C33(H33), C52(H52), C26(H26), C34(H34), C25(H25), C55(H55), C24(H24), C35(H35) 5.c Fitted hexagon refined as free rotating group: C7(C6,C5,C4,C3,C2), C8(C13,C12,C11,C10,C9) ; _shelx_res_file ; TITL hb_1285_9_1_scale_a.res in P4(1)2(1)2 hb_1285_9_1_scale.res created by SHELXL-2016/6 at 18:39:36 on 22-Oct-2020 REM Old TITL HB_1285_9_1_scale in P4(1)2(1)2 REM SHELXT solution in P4(1)2(1)2 REM R1 0.081, Rweak 0.025, Alpha 0.011, Orientation as input REM Flack x = -0.019 ( 0.007 ) from Parsons' quotients REM Formula found by SHELXT: C58 Cl7 Rh2 CELL 1.54184 14.9951 14.9951 26.1521 90 90 90 ZERR 4 0.0001 0.0001 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5-Y,0.5+X,0.25+Z SYMM 0.5+Y,0.5-X,0.75+Z SYMM 0.5-X,0.5+Y,0.25-Z SYMM 0.5+X,0.5-Y,0.75-Z SYMM +Y,+X,-Z SYMM -Y,-X,0.5-Z SFAC C H Cl P Rh UNIT 240 202 14 16 8 DELU 0.005 0.005 C7 C5 C3 C6 C4 C2 DELU 0.002 0.002 C10 C8 C12 C13 C11 C9 DELU 0.005 0.005 Rh1 C8 SIMU 0.02 0.04 1.7 C7 C5 C3 C6 C4 C2 SIMU 0.01 0.02 1.7 C10 C8 C12 C13 C11 C9 L.S. 4 0 0 PLAN 20 BOND $H list 4 fmap 2 53 ACTA OMIT 1 2 3 OMIT -1 3 2 OMIT -1 2 3 OMIT 2 2 4 OMIT 0 3 1 OMIT 1 1 2 OMIT 1 2 1 OMIT -1 2 1 OMIT 0 2 4 OMIT 0 2 0 OMIT 1 3 6 OMIT 2 2 1 OMIT 1 1 3 OMIT 1 1 6 OMIT 2 3 0 OMIT -1 3 6 OMIT 2 2 0 OMIT 0 1 5 OMIT 0 1 3 REM REM REM WGHT 0.060200 2.780500 FVAR 0.35894 RH1 5 0.721031 0.628227 0.452283 11.00000 0.02291 0.02467 = 0.01746 0.00132 0.00147 0.00172 CL2 3 0.766631 0.766631 0.500000 10.50000 0.03017 0.03017 = 0.02794 0.00334 -0.00334 -0.00909 CL1 3 0.855248 0.628815 0.396526 11.00000 0.02745 0.03955 = 0.02496 0.00045 0.00564 -0.00065 PART -3 CL3 3 0.654262 0.506676 0.411625 10.25000 0.03848 0.01905 = 0.02704 -0.00504 -0.00616 -0.00283 PART 0 P1 4 0.796122 0.530935 0.508918 11.00000 0.02291 0.02337 = 0.01977 0.00148 0.00124 0.00132 P2 4 0.720229 0.635797 0.602847 11.00000 0.02376 0.02464 = 0.01592 0.00052 -0.00104 -0.00023 PART -1 AFIX 66 C7 1 0.503596 0.499323 0.483209 10.50000 0.02864 0.03205 = 0.09380 -0.00667 0.01145 -0.00653 AFIX 43 H7 2 0.464444 0.511891 0.509831 10.50000 -1.20000 AFIX 65 C6 1 0.485357 0.429732 0.449692 10.50000 0.03904 0.03670 = 0.12241 -0.01493 0.00161 -0.00885 AFIX 43 H6 2 0.434002 0.395738 0.453888 10.50000 -1.20000 AFIX 65 C5 1 0.543875 0.410949 0.409902 10.50000 0.05047 0.03483 = 0.07702 -0.01307 -0.01877 -0.00427 AFIX 43 H5 2 0.531671 0.364387 0.387477 10.50000 -1.20000 AFIX 65 C4 1 0.620631 0.461757 0.403630 10.50000 0.05540 0.03148 = 0.03434 -0.00670 -0.01173 -0.00245 AFIX 43 H4 2 0.659782 0.449189 0.377008 10.50000 -1.20000 AFIX 65 C3 1 0.638870 0.531349 0.437147 10.50000 0.03548 0.02491 = 0.02620 -0.00429 -0.00593 0.00113 C2 1 0.580354 0.550133 0.476936 10.50000 0.03151 0.02406 = 0.04049 -0.00190 0.00261 -0.00079 AFIX 0 PART 0 C44 1 0.989220 0.748587 0.657910 11.00000 0.02968 0.07539 = 0.05429 -0.01385 -0.00838 -0.01410 AFIX 43 H44 2 1.042981 0.771422 0.669865 11.00000 -1.20000 AFIX 0 C31 1 0.914130 0.544420 0.523247 11.00000 0.02252 0.04239 = 0.01999 0.00503 0.00631 0.00200 C53 1 0.578162 0.647275 0.734864 11.00000 0.08905 0.04802 = 0.04797 0.00140 0.03876 0.01329 AFIX 43 H53 2 0.541439 0.688951 0.750682 11.00000 -1.20000 AFIX 0 C54 1 0.594152 0.566868 0.758034 11.00000 0.06499 0.05993 = 0.03458 0.00844 0.02322 0.00271 AFIX 43 H54 2 0.568188 0.553787 0.789446 11.00000 -1.20000 AFIX 0 C36 1 0.958680 0.474294 0.545935 11.00000 0.03161 0.04925 = 0.03852 0.01812 0.00191 0.00248 AFIX 43 H36 2 0.929979 0.419968 0.550783 11.00000 -1.20000 AFIX 0 C14 1 0.745069 0.527136 0.572743 11.00000 0.02661 0.02625 = 0.02222 0.00126 0.00066 -0.00033 AFIX 23 H14A 2 0.784623 0.494295 0.595255 11.00000 -1.20000 H14B 2 0.689888 0.493642 0.570330 11.00000 -1.20000 AFIX 66 PART -2 C8 1 0.659805 0.516858 0.410417 10.25000 0.04320 0.02600 = 0.03136 -0.00599 -0.00260 0.00477 C13 1 0.568420 0.501349 0.409862 10.25000 0.04301 0.02460 = 0.03065 -0.00137 -0.00540 0.00476 AFIX 43 H13 2 0.530259 0.538912 0.427805 10.25000 -1.20000 AFIX 65 C12 1 0.534072 0.429698 0.382490 10.25000 0.04803 0.03204 = 0.03113 -0.00458 -0.00290 -0.00062 AFIX 43 H12 2 0.472929 0.419322 0.382119 10.25000 -1.20000 AFIX 65 C11 1 0.591108 0.373555 0.355672 10.25000 0.05606 0.04019 = 0.03005 -0.01152 -0.00384 0.00229 AFIX 43 H11 2 0.568126 0.325616 0.337359 10.25000 -1.20000 AFIX 65 C10 1 0.682493 0.389063 0.356227 10.25000 0.05504 0.03551 = 0.03371 -0.01183 0.00053 0.00689 AFIX 43 H10 2 0.720653 0.351500 0.338284 10.25000 -1.20000 AFIX 65 C9 1 0.716843 0.460714 0.383599 10.25000 0.04822 0.02741 = 0.03473 -0.00512 0.00398 0.00461 AFIX 43 H9 2 0.777985 0.471090 0.383970 10.25000 -1.20000 AFIX 0 PART 0 C41 1 0.828095 0.681031 0.622790 11.00000 0.02699 0.03767 = 0.01937 -0.00401 -0.00168 -0.00404 C46 1 0.889100 0.624701 0.647088 11.00000 0.03466 0.04318 = 0.03255 0.00321 -0.00358 0.00055 AFIX 43 H46 2 0.875544 0.564710 0.651666 11.00000 -1.20000 AFIX 0 C1 1 0.624763 0.624763 0.500000 10.50000 0.02685 0.02685 = 0.01894 0.00598 -0.00598 0.00021 C32 1 0.957015 0.625167 0.514613 11.00000 0.02789 0.04198 = 0.02803 0.00509 0.00092 -0.00109 AFIX 43 H32 2 0.927138 0.671680 0.498492 11.00000 -1.20000 AFIX 0 C43 1 0.929786 0.804494 0.634054 11.00000 0.04527 0.04477 = 0.03733 -0.01067 -0.00053 -0.01277 AFIX 43 H43 2 0.943838 0.864301 0.629186 11.00000 -1.20000 AFIX 0 C51 1 0.669966 0.604548 0.663856 11.00000 0.02797 0.03378 = 0.02245 -0.00257 0.00155 -0.00424 C22 1 0.841213 0.392575 0.444501 11.00000 0.08261 0.04382 = 0.06410 -0.01143 0.03947 -0.01385 AFIX 43 H22 2 0.883036 0.432574 0.431712 11.00000 -1.20000 AFIX 0 C56 1 0.685670 0.522845 0.687135 11.00000 0.03104 0.03908 = 0.02411 0.00516 0.00472 0.00589 AFIX 43 H56 2 0.720669 0.480204 0.670884 11.00000 -1.20000 AFIX 0 C45 1 0.970559 0.658571 0.664521 11.00000 0.03240 0.07136 = 0.05307 0.00287 -0.01490 0.00295 AFIX 43 H45 2 1.011716 0.621274 0.680344 11.00000 -1.20000 AFIX 0 C21 1 0.788942 0.416024 0.486716 11.00000 0.03969 0.02655 = 0.02688 0.00126 0.00234 0.00337 C23 1 0.830892 0.311080 0.422072 11.00000 0.11158 0.04367 = 0.07467 -0.02349 0.04626 -0.00112 AFIX 43 H23 2 0.864138 0.296849 0.393182 11.00000 -1.20000 AFIX 0 C42 1 0.847293 0.770525 0.616997 11.00000 0.03623 0.03502 = 0.02330 -0.00420 -0.00134 -0.00145 AFIX 43 H42 2 0.805852 0.808367 0.601858 11.00000 -1.20000 AFIX 0 C33 1 1.045609 0.635915 0.530391 11.00000 0.02410 0.06453 = 0.04026 0.01475 -0.00114 -0.00668 AFIX 43 H33 2 1.074679 0.689937 0.525164 11.00000 -1.20000 AFIX 0 C52 1 0.616196 0.666556 0.688335 11.00000 0.06244 0.03536 = 0.03556 0.00542 0.01711 0.00444 AFIX 43 H52 2 0.605791 0.721651 0.673134 11.00000 -1.20000 AFIX 0 C26 1 0.729168 0.354713 0.505285 11.00000 0.05332 0.02917 = 0.03183 -0.00070 0.00671 -0.00177 AFIX 43 H26 2 0.694260 0.369336 0.533457 11.00000 -1.20000 AFIX 0 C34 1 1.089477 0.566353 0.553634 11.00000 0.02164 0.09723 = 0.04411 0.02492 -0.00602 -0.00039 AFIX 43 H34 2 1.148262 0.573732 0.564150 11.00000 -1.20000 AFIX 0 C25 1 0.719939 0.272831 0.483267 11.00000 0.07877 0.02837 = 0.03844 -0.00027 0.00601 -0.00786 AFIX 43 H25 2 0.678725 0.232279 0.496133 11.00000 -1.20000 AFIX 0 C55 1 0.649203 0.505197 0.734399 11.00000 0.05038 0.04750 = 0.03472 0.01634 0.01038 0.00760 AFIX 43 H55 2 0.661650 0.451399 0.750589 11.00000 -1.20000 AFIX 0 C24 1 0.772550 0.250383 0.441460 11.00000 0.11128 0.02949 = 0.04947 -0.01189 0.02039 -0.00308 AFIX 43 H24 2 0.767896 0.194078 0.426790 11.00000 -1.20000 AFIX 0 C35 1 1.047088 0.485246 0.561594 11.00000 0.03350 0.08179 = 0.05525 0.03560 -0.00166 0.00620 AFIX 43 H35 2 1.077339 0.438492 0.577249 11.00000 -1.20000 AFIX 0 HKLF 4 REM hb_1285_9_1_scale_a.res in P4(1)2(1)2 REM R1 = 0.0340 for 5367 Fo > 4sig(Fo) and 0.0353 for all 5538 data REM 365 parameters refined using 97 restraints END WGHT 0.0602 2.7805 REM Highest difference peak 0.927, deepest hole -0.679, 1-sigma level 0.095 Q1 1 0.6308 0.2193 0.2951 11.00000 0.05 0.93 Q2 1 0.7626 0.3414 0.2724 11.00000 0.05 0.62 Q3 1 0.7452 0.3359 0.2815 11.00000 0.05 0.61 Q4 1 0.5865 0.2324 0.3259 11.00000 0.05 0.61 Q5 1 0.7240 0.3308 0.2898 11.00000 0.05 0.56 Q6 1 0.8195 0.2834 0.2498 11.00000 0.05 0.53 Q7 1 0.6563 0.2774 0.3055 11.00000 0.05 0.51 Q8 1 0.5764 0.3115 0.3458 11.00000 0.05 0.48 Q9 1 0.6320 0.2950 0.3166 11.00000 0.05 0.46 Q10 1 0.4857 0.3415 0.3951 11.00000 0.05 0.38 Q11 1 0.2898 0.2898 0.5000 10.50000 0.05 0.38 Q12 1 0.9244 0.7031 0.4907 11.00000 0.05 0.36 Q13 1 0.8474 0.6201 0.4904 11.00000 0.05 0.33 Q14 1 0.7321 0.7010 0.4483 11.00000 0.05 0.33 Q15 1 0.7960 0.6318 0.4594 11.00000 0.05 0.32 Q16 1 0.7181 0.5944 0.5436 11.00000 0.05 0.31 Q17 1 0.5816 0.6161 0.4896 11.00000 0.05 0.31 Q18 1 0.8680 0.7438 0.4788 11.00000 0.05 0.30 Q19 1 0.8464 0.7636 0.4895 11.00000 0.05 0.30 Q20 1 0.8602 0.7261 0.4600 11.00000 0.05 0.30 ; _shelx_res_checksum 9543 _ins_header ; TITL HB_1285_9_1_scale in P4(1)2(1)2 REM P4(1)2(1)2 (#92 in standard setting) CELL 1.54184 14.995112 14.995112 26.152081 90.0000 90.0000 90.0000 ZERR 4.00 0.000118 0.000118 0.000369 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM -y+1/2, x+1/2, z+1/4 SYMM y+1/2,-x+1/2, z+3/4 SYMM -x+1/2, y+1/2,-z+1/4 SYMM x+1/2,-y+1/2,-z+3/4 SYMM y, x,-z SYMM -y,-x,-z+1/2 SFAC C H P Cl Rh UNIT 240.00 200.00 16.00 12.00 8.00 TREF HKLF 4 END ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.172 _oxdiff_exptl_absorpt_empirical_full_min 0.663 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -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 Rh1 Rh 0.72103(2) 0.62823(3) 0.45228(2) 0.02168(13) Uani 1 1 d . U . . . Cl2 Cl 0.76663(9) 0.76663(9) 0.500000 0.0294(4) Uani 1 2 d S T P A . Cl1 Cl 0.85525(9) 0.62881(10) 0.39653(5) 0.0307(3) Uani 1 1 d . . . . . Cl3 Cl 0.6543(5) 0.5067(5) 0.4116(3) 0.0282(15) Uani 0.25 1 d . . . A -3 P1 P 0.79612(9) 0.53093(9) 0.50892(5) 0.0220(3) Uani 1 1 d . . . . . P2 P 0.72023(9) 0.63580(9) 0.60285(4) 0.0214(3) Uani 1 1 d . . . . . C7 C 0.5036(6) 0.4993(6) 0.4832(4) 0.051(4) Uani 0.5 1 d . U . A -1 H7 H 0.464444 0.511891 0.509831 0.062 Uiso 0.5 1 calc R . . A -1 C6 C 0.4854(5) 0.4297(6) 0.4497(5) 0.066(4) Uani 0.5 1 d G U . A -1 H6 H 0.434002 0.395738 0.453888 0.079 Uiso 0.5 1 calc R . . A -1 C5 C 0.5439(7) 0.4109(6) 0.4099(4) 0.054(3) Uani 0.5 1 d G U . A -1 H5 H 0.531671 0.364387 0.387477 0.065 Uiso 0.5 1 calc R . . A -1 C4 C 0.6206(6) 0.4618(6) 0.4036(3) 0.040(3) Uani 0.5 1 d G U . A -1 H4 H 0.659782 0.449189 0.377008 0.048 Uiso 0.5 1 calc R . . A -1 C3 C 0.6389(5) 0.5313(5) 0.4371(3) 0.029(2) Uani 0.5 1 d G U . A -1 C2 C 0.5804(6) 0.5501(5) 0.4769(3) 0.032(2) Uani 0.5 1 d G U . A -1 C44 C 0.9892(5) 0.7486(6) 0.6579(3) 0.053(2) Uani 1 1 d . . . . . H44 H 1.042981 0.771422 0.669865 0.064 Uiso 1 1 calc R . . . . C31 C 0.9141(4) 0.5444(4) 0.5232(2) 0.0283(12) Uani 1 1 d . . . . . C53 C 0.5782(6) 0.6473(5) 0.7349(3) 0.062(2) Uani 1 1 d . . . . . H53 H 0.541439 0.688951 0.750682 0.074 Uiso 1 1 calc R . . . . C54 C 0.5942(6) 0.5669(6) 0.7580(3) 0.053(2) Uani 1 1 d . . . . . H54 H 0.568188 0.553787 0.789446 0.064 Uiso 1 1 calc R . . . . C36 C 0.9587(4) 0.4743(5) 0.5459(3) 0.0398(15) Uani 1 1 d . . . . . H36 H 0.929979 0.419968 0.550783 0.048 Uiso 1 1 calc R . . . . C14 C 0.7451(4) 0.5271(4) 0.5727(2) 0.0250(11) Uani 1 1 d . . . . . H14A H 0.784623 0.494295 0.595255 0.030 Uiso 1 1 calc R . . . . H14B H 0.689888 0.493642 0.570330 0.030 Uiso 1 1 calc R . . . . C8 C 0.6598(12) 0.5169(11) 0.4104(8) 0.034(5) Uani 0.25 1 d . U . A -2 C13 C 0.5684(11) 0.5013(11) 0.4099(7) 0.033(4) Uani 0.25 1 d G U . A -2 H13 H 0.530259 0.538912 0.427805 0.039 Uiso 0.25 1 calc R . . A -2 C12 C 0.5341(9) 0.4297(12) 0.3825(7) 0.037(4) Uani 0.25 1 d G U . A -2 H12 H 0.472929 0.419322 0.382119 0.044 Uiso 0.25 1 calc R . . A -2 C11 C 0.5911(11) 0.3736(10) 0.3557(6) 0.042(4) Uani 0.25 1 d G U . A -2 H11 H 0.568126 0.325616 0.337359 0.051 Uiso 0.25 1 calc R . . A -2 C10 C 0.6825(11) 0.3891(11) 0.3562(6) 0.041(4) Uani 0.25 1 d G U . A -2 H10 H 0.720653 0.351500 0.338284 0.050 Uiso 0.25 1 calc R . . A -2 C9 C 0.7168(9) 0.4607(12) 0.3836(8) 0.037(4) Uani 0.25 1 d G U . A -2 H9 H 0.777985 0.471090 0.383970 0.044 Uiso 0.25 1 calc R . . A -2 C41 C 0.8281(4) 0.6810(4) 0.6228(2) 0.0280(12) Uani 1 1 d . . . . . C46 C 0.8891(4) 0.6247(5) 0.6471(2) 0.0368(13) Uani 1 1 d . . . . . H46 H 0.875544 0.564710 0.651666 0.044 Uiso 1 1 calc R . . . . C1 C 0.6248(4) 0.6248(4) 0.500000 0.0242(14) Uani 1 2 d S T P A . C32 C 0.9570(4) 0.6252(5) 0.5146(2) 0.0326(12) Uani 1 1 d . . . . . H32 H 0.927138 0.671680 0.498492 0.039 Uiso 1 1 calc R . . . . C43 C 0.9298(5) 0.8045(5) 0.6341(3) 0.0425(16) Uani 1 1 d . . . . . H43 H 0.943838 0.864301 0.629186 0.051 Uiso 1 1 calc R . . . . C51 C 0.6700(4) 0.6045(4) 0.6639(2) 0.0281(12) Uani 1 1 d . . . . . C22 C 0.8412(7) 0.3926(5) 0.4445(3) 0.064(3) Uani 1 1 d . . . . . H22 H 0.883036 0.432574 0.431712 0.076 Uiso 1 1 calc R . . . . C56 C 0.6857(4) 0.5228(4) 0.6871(2) 0.0314(13) Uani 1 1 d . . . . . H56 H 0.720669 0.480204 0.670884 0.038 Uiso 1 1 calc R . . . . C45 C 0.9706(5) 0.6586(6) 0.6645(3) 0.0523(19) Uani 1 1 d . . . . . H45 H 1.011716 0.621274 0.680344 0.063 Uiso 1 1 calc R . . . . C21 C 0.7889(4) 0.4160(4) 0.4867(2) 0.0310(12) Uani 1 1 d . . . . . C23 C 0.8309(8) 0.3111(6) 0.4221(4) 0.077(3) Uani 1 1 d . . . . . H23 H 0.864138 0.296849 0.393182 0.092 Uiso 1 1 calc R . . . . C42 C 0.8473(4) 0.7705(4) 0.6170(2) 0.0315(12) Uani 1 1 d . . . . . H42 H 0.805852 0.808367 0.601858 0.038 Uiso 1 1 calc R . . . . C33 C 1.0456(4) 0.6359(5) 0.5304(3) 0.0430(16) Uani 1 1 d . . . . . H33 H 1.074679 0.689937 0.525164 0.052 Uiso 1 1 calc R . . . . C52 C 0.6162(5) 0.6666(5) 0.6883(3) 0.0444(17) Uani 1 1 d . . . . . H52 H 0.605791 0.721651 0.673134 0.053 Uiso 1 1 calc R . . . . C26 C 0.7292(5) 0.3547(4) 0.5053(2) 0.0381(14) Uani 1 1 d . . . . . H26 H 0.694260 0.369336 0.533457 0.046 Uiso 1 1 calc R . . . . C34 C 1.0895(4) 0.5664(6) 0.5536(3) 0.054(2) Uani 1 1 d . . . . . H34 H 1.148262 0.573732 0.564150 0.065 Uiso 1 1 calc R . . . . C25 C 0.7199(6) 0.2728(4) 0.4833(3) 0.0485(17) Uani 1 1 d . . . . . H25 H 0.678725 0.232279 0.496133 0.058 Uiso 1 1 calc R . . . . C55 C 0.6492(5) 0.5052(5) 0.7344(2) 0.0442(17) Uani 1 1 d . . . . . H55 H 0.661650 0.451399 0.750589 0.053 Uiso 1 1 calc R . . . . C24 C 0.7726(7) 0.2504(5) 0.4415(3) 0.063(2) Uani 1 1 d . . . . . H24 H 0.767896 0.194078 0.426790 0.076 Uiso 1 1 calc R . . . . C35 C 1.0471(5) 0.4852(6) 0.5616(3) 0.057(2) Uani 1 1 d . . . . . H35 H 1.077339 0.438492 0.577249 0.068 Uiso 1 1 calc R . . . . 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 Rh1 0.0229(2) 0.0247(2) 0.01746(18) 0.00132(15) 0.00147(15) 0.00172(15) Cl2 0.0302(6) 0.0302(6) 0.0279(9) 0.0033(5) -0.0033(5) -0.0091(8) Cl1 0.0275(6) 0.0396(7) 0.0250(6) 0.0005(5) 0.0056(5) -0.0006(6) Cl3 0.038(4) 0.019(3) 0.027(3) -0.005(2) -0.006(3) -0.003(3) P1 0.0229(6) 0.0234(6) 0.0198(6) 0.0015(5) 0.0012(5) 0.0013(5) P2 0.0238(6) 0.0246(6) 0.0159(5) 0.0005(5) -0.0010(5) -0.0002(5) C7 0.029(6) 0.032(6) 0.094(11) -0.007(7) 0.011(7) -0.007(4) C6 0.039(7) 0.037(7) 0.122(12) -0.015(7) 0.002(7) -0.009(5) C5 0.050(7) 0.035(7) 0.077(9) -0.013(7) -0.019(6) -0.004(5) C4 0.055(7) 0.031(6) 0.034(6) -0.007(5) -0.012(5) -0.002(6) C3 0.035(6) 0.025(5) 0.026(5) -0.004(4) -0.006(4) 0.001(4) C2 0.032(5) 0.024(5) 0.040(6) -0.002(4) 0.003(5) -0.001(4) C44 0.030(3) 0.075(6) 0.054(4) -0.014(4) -0.008(3) -0.014(3) C31 0.023(3) 0.042(3) 0.020(2) 0.005(2) 0.006(2) 0.002(2) C53 0.089(6) 0.048(4) 0.048(4) 0.001(4) 0.039(4) 0.013(4) C54 0.065(5) 0.060(5) 0.035(3) 0.008(3) 0.023(3) 0.003(4) C36 0.032(3) 0.049(4) 0.039(3) 0.018(3) 0.002(3) 0.002(3) C14 0.027(3) 0.026(3) 0.022(2) 0.001(2) 0.001(2) 0.000(2) C8 0.043(9) 0.026(10) 0.031(11) -0.006(7) -0.003(9) 0.005(7) C13 0.043(9) 0.025(8) 0.031(8) -0.001(6) -0.005(7) 0.005(7) C12 0.048(8) 0.032(9) 0.031(8) -0.005(7) -0.003(8) -0.001(6) C11 0.056(8) 0.040(9) 0.030(8) -0.012(7) -0.004(8) 0.002(7) C10 0.055(8) 0.036(8) 0.034(8) -0.012(6) 0.001(8) 0.007(7) C9 0.048(8) 0.027(8) 0.035(9) -0.005(7) 0.004(8) 0.005(7) C41 0.027(3) 0.038(3) 0.019(2) -0.004(2) -0.002(2) -0.004(2) C46 0.035(3) 0.043(3) 0.033(3) 0.003(3) -0.004(2) 0.001(3) C1 0.027(2) 0.027(2) 0.019(3) 0.006(2) -0.006(2) 0.000(3) C32 0.028(3) 0.042(3) 0.028(3) 0.005(3) 0.001(2) -0.001(3) C43 0.045(4) 0.045(4) 0.037(3) -0.011(3) -0.001(3) -0.013(3) C51 0.028(3) 0.034(3) 0.022(2) -0.003(2) 0.002(2) -0.004(2) C22 0.083(6) 0.044(4) 0.064(5) -0.011(4) 0.039(5) -0.014(4) C56 0.031(3) 0.039(3) 0.024(3) 0.005(2) 0.005(2) 0.006(3) C45 0.032(4) 0.071(5) 0.053(4) 0.003(4) -0.015(3) 0.003(3) C21 0.040(3) 0.027(3) 0.027(3) 0.001(2) 0.002(2) 0.003(2) C23 0.112(8) 0.044(4) 0.075(6) -0.023(4) 0.046(6) -0.001(5) C42 0.036(3) 0.035(3) 0.023(3) -0.004(2) -0.001(2) -0.001(3) C33 0.024(3) 0.065(4) 0.040(3) 0.015(3) -0.001(3) -0.007(3) C52 0.062(5) 0.035(3) 0.036(3) 0.005(3) 0.017(3) 0.004(3) C26 0.053(4) 0.029(3) 0.032(3) -0.001(2) 0.007(3) -0.002(3) C34 0.022(3) 0.097(6) 0.044(4) 0.025(4) -0.006(3) 0.000(3) C25 0.079(5) 0.028(3) 0.038(3) 0.000(3) 0.006(4) -0.008(3) C55 0.050(4) 0.048(4) 0.035(3) 0.016(3) 0.010(3) 0.008(3) C24 0.111(7) 0.029(3) 0.049(4) -0.012(3) 0.020(5) -0.003(4) C35 0.033(4) 0.082(6) 0.055(5) 0.036(4) -0.002(3) 0.006(4) 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' Cl Cl 0.3639 0.7018 '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' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -9 -8 0.0980 1 9 8 0.0980 9 -1 -4 0.0955 -9 1 4 0.0955 4 0 15 0.0799 1 7 -13 0.0431 -6 -3 -13 0.0730 -4 -8 5 0.0990 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 Cl2 Rh1 Rh1 50.84(3) . 7_556 ? Cl1 Rh1 Rh1 144.46(3) . 7_556 ? Cl1 Rh1 Cl2 93.90(4) . . ? Cl1 Rh1 C2 146.84(15) . . ? Cl3 Rh1 Rh1 120.76(19) . 7_556 ? Cl3 Rh1 Cl2 170.36(18) . . ? Cl3 Rh1 Cl1 94.7(2) . . ? Cl3 Rh1 P1 90.45(19) . . ? Cl3 Rh1 P2 86.91(19) . 7_556 ? P1 Rh1 Rh1 89.24(3) . 7_556 ? P1 Rh1 Cl2 93.95(3) . . ? P1 Rh1 Cl1 89.09(5) . . ? P1 Rh1 P2 175.74(5) . 7_556 ? P1 Rh1 C2 87.2(2) . . ? P2 Rh1 Rh1 89.24(3) 7_556 7_556 ? P2 Rh1 Cl2 88.17(3) 7_556 . ? P2 Rh1 Cl1 94.46(5) 7_556 . ? P2 Rh1 C2 88.5(2) 7_556 . ? C3 Rh1 Rh1 102.1(2) . 7_556 ? C3 Rh1 Cl2 152.7(2) . . ? C3 Rh1 Cl1 113.3(2) . . ? C3 Rh1 P1 88.2(3) . . ? C3 Rh1 P2 88.2(3) . 7_556 ? C3 Rh1 C2 33.64(14) . . ? C2 Rh1 Rh1 68.45(15) . 7_556 ? C2 Rh1 Cl2 119.22(15) . . ? C8 Rh1 Rh1 122.7(5) . 7_556 ? C8 Rh1 Cl2 170.8(5) . . ? C8 Rh1 Cl1 92.8(5) . . ? C8 Rh1 P1 92.4(6) . . ? C8 Rh1 P2 85.1(6) . 7_556 ? C1 Rh1 Rh1 33.6(2) . 7_556 ? C1 Rh1 Cl2 84.5(2) . . ? C1 Rh1 Cl1 174.90(7) . . ? C1 Rh1 Cl3 87.3(3) . . ? C1 Rh1 P1 86.21(4) . . ? C1 Rh1 P2 90.33(3) . 7_556 ? C1 Rh1 C3 68.5(3) . . ? C1 Rh1 C2 34.9(2) . . ? C1 Rh1 C8 89.4(6) . . ? Rh1 Cl2 Rh1 78.33(5) . 7_556 ? C31 P1 Rh1 121.56(19) . . ? C31 P1 C14 102.8(2) . . ? C31 P1 C21 103.2(3) . . ? C14 P1 Rh1 112.94(18) . . ? C21 P1 Rh1 110.85(19) . . ? C21 P1 C14 103.6(3) . . ? C14 P2 Rh1 109.50(18) . 7_556 ? C41 P2 Rh1 119.2(2) . 7_556 ? C41 P2 C14 105.7(3) . . ? C51 P2 Rh1 115.5(2) . 7_556 ? C51 P2 C14 103.3(3) . . ? C51 P2 C41 102.2(3) . . ? C6 C7 H7 120.0 . . ? C6 C7 C2 120.0 . . ? C2 C7 H7 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C5 H5 120.0 . . ? C6 C5 C4 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C4 H4 120.0 . . ? C5 C4 C3 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C3 Rh1 144.4(5) . . ? C2 C3 Rh1 95.5(5) . . ? C2 C3 C4 120.0 . . ? C7 C2 Rh1 170.7(4) . . ? C7 C2 C1 139.6(6) . . ? C3 C2 Rh1 50.8(3) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 100.4(6) . . ? C1 C2 Rh1 49.5(3) . . ? C43 C44 H44 119.4 . . ? C43 C44 C45 121.3(6) . . ? C45 C44 H44 119.4 . . ? C36 C31 P1 118.3(5) . . ? C36 C31 C32 120.7(6) . . ? C32 C31 P1 120.9(4) . . ? C54 C53 H53 119.9 . . ? C54 C53 C52 120.3(7) . . ? C52 C53 H53 119.9 . . ? C53 C54 H54 120.2 . . ? C53 C54 C55 119.6(6) . . ? C55 C54 H54 120.2 . . ? C31 C36 H36 120.1 . . ? C31 C36 C35 119.7(7) . . ? C35 C36 H36 120.1 . . ? P1 C14 P2 116.3(3) . . ? P1 C14 H14A 108.2 . . ? P1 C14 H14B 108.2 . . ? P2 C14 H14A 108.2 . . ? P2 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C13 C8 Rh1 123.0(9) . . ? C13 C8 C9 120.0 . . ? C9 C8 Rh1 117.0(9) . . ? C8 C13 H13 120.0 . . ? C8 C13 C12 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C46 C41 P2 118.9(5) . . ? C42 C41 P2 120.9(5) . . ? C42 C41 C46 120.0(6) . . ? C41 C46 H46 120.0 . . ? C41 C46 C45 120.0(7) . . ? C45 C46 H46 120.0 . . ? Rh1 C1 Rh1 112.7(4) . 7_556 ? C2 C1 Rh1 151.3(5) . 7_556 ? C2 C1 Rh1 95.6(3) . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.4(6) . . ? C33 C32 H32 120.3 . . ? C44 C43 H43 120.2 . . ? C44 C43 C42 119.5(7) . . ? C42 C43 H43 120.2 . . ? C56 C51 P2 122.7(4) . . ? C52 C51 P2 118.1(5) . . ? C52 C51 C56 119.2(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C23 C22 C21 120.1(7) . . ? C51 C56 H56 120.1 . . ? C55 C56 C51 119.7(6) . . ? C55 C56 H56 120.1 . . ? C44 C45 C46 119.2(7) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? C22 C21 P1 117.1(5) . . ? C26 C21 P1 124.0(5) . . ? C26 C21 C22 118.5(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 C22 120.8(8) . . ? C24 C23 H23 119.6 . . ? C41 C42 C43 119.9(6) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C32 C33 H33 120.1 . . ? C34 C33 C32 119.8(7) . . ? C34 C33 H33 120.1 . . ? C53 C52 C51 120.6(6) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C21 C26 H26 119.3 . . ? C25 C26 C21 121.3(6) . . ? C25 C26 H26 119.3 . . ? C33 C34 H34 119.6 . . ? C33 C34 C35 120.8(6) . . ? C35 C34 H34 119.6 . . ? C26 C25 H25 120.2 . . ? C26 C25 C24 119.5(7) . . ? C24 C25 H25 120.2 . . ? C54 C55 H55 119.7 . . ? C56 C55 C54 120.6(6) . . ? C56 C55 H55 119.7 . . ? C23 C24 C25 119.8(7) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C36 C35 H35 120.2 . . ? C34 C35 C36 119.6(7) . . ? C34 C35 H35 120.2 . . ? 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 Rh1 Rh1 3.1785(7) 7_556 ? Rh1 Cl2 2.5164(15) . ? Rh1 Cl1 2.4853(13) . ? Rh1 Cl3 2.336(7) . ? Rh1 P1 2.3643(13) . ? Rh1 P2 2.3697(13) 7_556 ? Rh1 C3 1.945(7) . ? Rh1 C2 2.497(8) . ? Rh1 C8 2.198(12) . ? Rh1 C1 1.909(4) . ? P1 C31 1.820(6) . ? P1 C14 1.837(5) . ? P1 C21 1.821(6) . ? P2 C14 1.848(6) . ? P2 C41 1.830(6) . ? P2 C51 1.826(6) . ? C7 H7 0.9300 . ? C7 C6 1.3900 . ? C7 C2 1.3900 . ? C6 H6 0.9300 . ? C6 C5 1.3900 . ? C5 H5 0.9300 . ? C5 C4 1.3900 . ? C4 H4 0.9300 . ? C4 C3 1.3900 . ? C3 C2 1.3900 . ? C2 C1 1.435(9) . ? C44 H44 0.9300 . ? C44 C43 1.373(11) . ? C44 C45 1.389(12) . ? C31 C36 1.380(8) . ? C31 C32 1.389(9) . ? C53 H53 0.9300 . ? C53 C54 1.371(11) . ? C53 C52 1.375(9) . ? C54 H54 0.9300 . ? C54 C55 1.385(10) . ? C36 H36 0.9300 . ? C36 C35 1.397(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C8 C13 1.3900 . ? C8 C9 1.3900 . ? C13 H13 0.9300 . ? C13 C12 1.3900 . ? C12 H12 0.9300 . ? C12 C11 1.3900 . ? C11 H11 0.9300 . ? C11 C10 1.3900 . ? C10 H10 0.9300 . ? C10 C9 1.3900 . ? C9 H9 0.9300 . ? C41 C46 1.398(9) . ? C41 C42 1.381(8) . ? C46 H46 0.9300 . ? C46 C45 1.399(9) . ? C32 H32 0.9300 . ? C32 C33 1.400(8) . ? C43 H43 0.9300 . ? C43 C42 1.410(9) . ? C51 C56 1.388(8) . ? C51 C52 1.387(9) . ? C22 H22 0.9300 . ? C22 C21 1.399(9) . ? C22 C23 1.364(11) . ? C56 H56 0.9300 . ? C56 C55 1.377(8) . ? C45 H45 0.9300 . ? C21 C26 1.373(9) . ? C23 H23 0.9300 . ? C23 C24 1.360(12) . ? C42 H42 0.9300 . ? C33 H33 0.9300 . ? C33 C34 1.375(10) . ? C52 H52 0.9300 . ? C26 H26 0.9300 . ? C26 C25 1.363(9) . ? C34 H34 0.9300 . ? C34 C35 1.388(12) . ? C25 H25 0.9300 . ? C25 C24 1.390(11) . ? C55 H55 0.9300 . ? C24 H24 0.9300 . ? C35 H35 0.9300 . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.8252 -8.6566 -7.5814 0.2208 -0.5264 -0.8211 0.8252 8.6566 7.5814 -0.2208 0.5264 0.8211 9.3095 -1.3994 -4.2870 0.3450 -0.8332 0.4322 -9.3095 1.3994 4.2870 -0.3450 0.8332 -0.4322 4.4038 -0.3589 15.1355 -0.8046 -0.3330 0.4916 0.5249 6.5524 -12.5558 0.8704 0.3624 0.3332 -5.6975 -2.5514 -13.0157 0.5991 0.2469 -0.7616 -4.0313 -8.3703 5.0850 -0.5380 -0.2256 -0.8122 loop_ _hkl_oxdiff_h _hkl_oxdiff_k _hkl_oxdiff_l _hkl_oxdiff_f2 _hkl_oxdiff_sig _hkl_oxdiff_ba 0 0 -3 747.043 129.664 1 0 0 -4 681049. 15041.2 1 0 0 -5 1213.34 205.450 1 0 0 -6 663.236 201.513 1 0 0 -7 861.017 235.483 1 0 0 -8 21302.2 1053.78 1 0 0 -9 218.817 199.246 1 0 0 -10 43.1476 171.392 1 0 0 -11 207.739 187.680 1 0 0 -12 6285.82 678.721 1 0 0 -13 245.960 249.706 1 0 0 -14 -235.555 288.330 1 0 0 -15 686.631 298.578 1 0 0 -16 90803.9 3533.44 1 0 0 -17 688.001 347.936 1 0 0 24 2677.50 698.002 5 0 0 25 -141.616 400.365 5 0 0 26 -391.603 452.027 5 0 0 27 156.270 295.575 5 0 0 28 24203.9 1732.87 5 0 0 29 -146.412 319.986 5 0 0 30 -104.849 275.366 5 0 1 -2 348875. 8073.56 1 1 0 -2 374869. 8076.09 1 0 1 -3 312824. 7300.59 1 1 0 -3 335824. 7291.37 1 -1 0 -3 314202. 7144.82 1 0 -1 -4 29155.2 926.289 1 -1 0 -4 26994.3 935.414 1 1 0 -4 30106.5 1034.43 1 0 1 -4 27849.1 1043.47 1 1 0 -5 186349. 4478.04 1 0 -1 -5 180423. 4325.76 1 0 1 -5 181836. 4510.74 1 -1 0 -5 172473. 4351.41 1 0 1 -6 191712. 4833.96 1 0 -1 -6 192364. 4644.82 1 1 0 -6 191737. 4784.89 1 -1 0 -6 184480. 4669.50 1 -1 0 -7 120185. 3255.45 1 1 0 -7 118782. 3335.77 1 0 1 -7 121191. 3387.65 1 0 -1 -7 117410. 3201.42 1 0 1 -8 456011. 10706.1 1 1 0 -8 449551. 10659.7 1 -1 0 -8 456429. 10547.8 1 0 -1 -8 445823. 10489.8 1 0 1 -9 873.884 270.063 1 1 0 -9 2189.06 389.991 1 0 -1 -9 1880.98 335.825 1 -1 0 -9 1112.40 247.528 1 -1 0 -10 6631.16 612.798 1 1 0 -10 7008.71 672.471 1 0 -1 -10 6223.34 585.368 1 0 1 -10 6778.16 660.093 1 -1 0 -11 31976.7 1498.00 1 1 0 -11 29501.3 1526.76 1 0 -1 -11 31432.4 1487.55 1 0 1 -11 32252.2 1600.62 1 0 -1 -12 1342.51 341.432 1 1 0 -12 789.546 273.623 1 -1 0 -12 523.428 221.314 1 0 1 -12 481.723 249.993 1 1 0 -13 43793.0 2081.65 1 -1 0 -13 42637.5 1970.08 1 0 -1 -13 43638.7 1988.05 1 0 1 -13 45325.9 2108.26 1 1 0 -14 98259.4 3577.76 1 -1 0 -14 99681.8 3461.63 1 0 1 -14 95194.3 3553.63 1 1 0 -15 68890.6 2968.79 1 0 1 -15 69345.6 2951.37 1 -1 0 -15 68960.4 2824.29 1 0 1 -16 144515. 4942.84 1 -1 0 -16 146825. 4823.34 1 -1 0 -17 189255. 5914.12 1 0 1 -17 183879. 6038.33 1 0 1 -18 48748.0 2640.96 1 0 1 -19 327201. 9566.80 1 1 0 22 97674.2 4377.56 5 0 1 22 98433.0 4275.20 5 1 0 23 43651.1 2761.56 5 0 1 23 44647.7 2703.53 5 0 1 24 4852.09 858.879 5 -1 0 24 3248.58 755.928 5 1 0 24 3583.12 838.330 5 0 1 25 -313.578 454.722 5 0 -1 25 600.373 488.517 5 1 0 25 -370.772 472.452 5 -1 0 25 234.925 371.720 5 1 0 26 -404.256 479.381 5 0 1 26 322.857 326.859 5 -1 0 26 -57.8048 361.762 5 0 -1 26 14.4769 404.410 5 -1 0 27 658.111 353.960 5 0 -1 27 499.775 337.200 5 0 1 27 164.133 352.811 5 1 0 27 329.535 309.475 5 0 1 28 -237.092 421.466 5 0 -1 28 -15.5603 347.790 5 -1 0 28 -94.1659 316.417 5 1 0 28 -91.1119 334.453 5 1 0 29 936.576 374.237 5 0 -1 29 1286.81 412.257 5 0 -1 30 10740.7 987.020 5 1 0 30 11526.3 1022.41 5 1 0 31 39584.8 1802.34 5 0 -1 31 37569.6 1757.90 5 1 1 0 789.228 81.2036 1 1 1 -1 903877. 19627.2 1 1 1 -2 579375. 12796.9 1 1 1 -3 43171.0 1359.49 1 -1 -1 -3 44725.9 1103.51 1 -1 1 -3 42665.7 1291.76 1 1 1 -4 2094.85 275.190 1 -1 1 -4 2019.53 240.258 1 -1 -1 -4 1546.49 155.580 1 -1 -1 -5 319348. 7226.02 1 1 1 -5 317203. 7540.12 1 -1 1 -5 319863. 7477.84 1 -1 1 -6 9593.19 625.113 1 1 1 -6 9030.53 631.457 1 -1 -1 -6 9129.63 506.804 1 -1 -1 -7 130588. 3392.32 1 1 1 -7 134151. 3695.47 1 -1 1 -7 129383. 3619.10 1 -1 1 -8 15210.9 909.867 1 -1 -1 -8 15052.2 789.529 1 1 1 -8 16100.7 958.600 1 -1 1 -9 139191. 3955.43 1 1 1 -9 138443. 4021.01 1 -1 -1 -9 133482. 3718.45 1 -1 1 -10 12869.6 899.438 1 -1 -1 -10 12587.7 808.970 1 1 1 -10 13411.9 961.773 1 1 1 -11 925.829 298.610 1 -1 -1 -11 1250.71 278.884 1 -1 1 -12 12810.0 988.496 1 -1 -1 -12 12121.5 876.730 1 1 1 -12 10583.8 952.327 1 1 1 -13 114618. 3959.47 1 -1 -1 -13 113770. 3665.20 1 -1 1 -13 117750. 3883.09 1 -1 1 -14 398219. 10300.1 1 1 1 -14 394385. 10429.8 1 -1 -1 -14 402486. 10070.6 1 -1 -1 -15 74011.0 2898.61 1 1 1 -15 71889.5 3120.45 1 -1 1 -15 78871.4 3119.32 1 1 1 -16 2454.21 534.905 1 -1 1 -16 2977.31 573.940 1 1 1 -17 22448.9 1697.88 1 -1 1 -17 23605.6 1660.93 1 1 1 -18 320696. 9593.62 1 -1 1 -18 348658. 9559.73 1 -1 1 -19 293686. 8695.15 1 1 1 20 243.362 405.274 5 1 1 21 119214. 4858.86 5 1 1 22 188505. 6633.78 5 1 1 23 2900.26 766.686 5 -1 1 23 3165.48 705.228 5 1 1 24 13163.7 1466.43 5 -1 1 24 13758.9 1411.13 5 1 -1 24 12730.6 1451.35 5 -1 1 25 14119.5 1416.83 5 1 1 25 10824.4 1312.53 5 1 -1 25 10837.8 1337.01 5 -1 -1 26 9073.88 1144.17 5 1 1 26 8131.36 1111.15 5 1 -1 26 8713.59 1126.90 5 1 1 27 286.837 350.463 5 -1 -1 27 1145.13 416.675 5 1 -1 27 1401.49 437.772 5 1 -1 28 1559.21 409.065 5 1 1 28 2381.09 577.684 5 -1 -1 28 3326.10 653.994 5 -1 -1 29 5980.74 770.360 5 1 1 29 5332.14 763.617 5 1 -1 29 6425.68 849.789 5 1 -1 30 5218.01 700.441 5 -1 -1 30 4041.94 593.608 5 1 -1 31 8789.25 808.192 5 2 0 0 891451. 19249.3 2 0 2 1 725190. 15779.3 2 0 2 2 178820. 4039.33 2 0 2 -2 170810. 4182.07 1 0 2 -3 5743.61 414.176 1 -2 0 -4 2484.79 227.718 1 0 2 -4 2606.46 313.857 1 2 0 -5 71861.3 2170.16 1 -2 0 -5 69404.7 1967.81 1 0 2 -5 71497.4 2210.63 1 -2 0 -6 42015.8 1404.37 1 2 0 -6 41405.5 1556.40 1 0 2 -6 39236.2 1566.27 1 -2 0 -7 255719. 6215.72 1 0 2 -7 253364. 6479.49 1 2 0 -7 259628. 6446.15 1 2 0 -8 15611.2 966.692 1 -2 0 -8 17504.0 907.840 1 0 2 -8 16649.8 1011.60 1 0 2 -9 82000.5 2789.47 1 -2 0 -9 79813.2 2538.47 1 2 0 -9 80078.0 2738.50 1 2 0 -10 23232.5 1341.58 1 0 2 -10 25274.5 1387.73 1 -2 0 -10 27038.2 1279.55 1 -2 0 -11 108729. 3355.02 1 2 0 -11 107314. 3587.58 1 0 2 -11 106022. 3588.58 1 2 0 -12 58565.7 2485.40 1 0 2 -12 57970.3 2489.27 1 -2 0 -12 59851.3 2290.23 1 0 2 -13 34777.8 1878.94 1 -2 0 -13 32923.1 1657.88 1 0 2 -14 146035. 4834.15 1 -2 0 -14 145113. 4521.53 1 0 2 -15 581141. 14721.3 1 -2 0 -15 592460. 14356.3 1 -2 0 -16 39424.1 2052.60 1 0 2 -16 40417.9 2277.18 1 0 2 -17 192960. 6304.84 1 0 2 -18 150666. 5412.51 1 0 2 -19 19182.2 1680.36 1 0 2 -20 202595. 6920.31 1 0 2 20 205844. 6755.01 5 0 2 21 117472. 4700.79 5 2 0 21 118614. 4931.78 5 2 0 22 9962.92 1301.55 5 0 2 22 9767.92 1194.02 5 2 0 23 46955.0 2907.36 5 0 2 23 49423.3 2834.79 5 0 2 24 31105.5 2157.06 5 2 0 24 27858.3 2188.38 5 2 0 25 80.7963 406.466 5 -2 0 25 838.575 488.694 5 0 -2 26 38554.3 2485.65 5 -2 0 26 42513.4 2413.02 5 2 0 26 40064.1 2563.27 5 2 0 27 2677.37 670.583 5 0 -2 27 3037.88 664.021 5 0 -2 28 1458.21 518.312 5 2 0 28 796.091 338.396 5 2 0 29 18186.5 1433.46 5 0 -2 29 17535.7 1389.54 5 2 0 30 6343.08 782.047 5 0 -2 30 5699.76 726.079 5 2 0 31 1012.55 321.685 5 0 -2 31 1144.07 301.359 5 2 -1 31 176.518 242.333 5 -1 -2 30 13425.4 1080.05 5 2 -1 30 15094.5 1218.20 5 2 -1 29 9553.75 1055.89 5 -1 -2 29 10225.7 1021.26 5 1 2 28 15486.1 1332.80 5 -1 -2 28 15640.7 1364.32 5 2 -1 28 16439.9 1458.58 5 2 -1 27 2162.37 570.848 5 1 2 27 2631.46 591.045 5 -1 -2 27 2691.80 642.533 5 1 2 26 4222.85 793.192 5 2 -1 26 6942.64 1050.07 5 2 -1 25 24750.6 2063.47 5 1 2 25 25768.7 2000.76 5 1 2 24 34316.3 2385.87 5 2 -1 24 39932.7 2623.86 5 1 2 23 44568.9 2734.75 5 2 -1 23 44830.1 2846.05 5 2 -1 22 59159.9 3300.75 5 1 2 22 61940.6 3266.97 5 1 2 21 37373.7 2444.42 5 -1 2 -20 235514. 7684.49 1 1 2 20 245087. 7709.96 5 -1 2 -19 214542. 7002.15 1 -1 2 -18 208675. 6737.93 1 -1 2 -17 16567.7 1429.04 1 -1 2 -16 64989.8 2952.06 1 2 1 -16 61022.4 2991.84 1 2 1 -15 42947.8 2334.24 1 -1 2 -15 43900.5 2282.24 1 -2 -1 -14 72419.5 2689.69 1 2 1 -14 73305.5 3085.89 1 -1 2 -14 73196.5 3017.03 1 -2 -1 -13 248242. 6529.08 1 -1 2 -13 246946. 6974.04 1 2 1 -13 241670. 7009.75 1 -1 2 -12 166265. 5054.28 1 2 1 -12 165843. 5144.25 1 -2 -1 -12 171028. 4688.59 1 -1 2 -11 31411.0 1638.76 1 2 1 -11 30922.3 1652.74 1 -2 -1 -11 31629.5 1397.53 1 -2 -1 -10 970.722 231.563 1 -1 2 -10 942.313 289.734 1 2 1 -10 1113.09 319.689 1 2 1 -9 94402.1 3122.60 1 -2 -1 -9 96181.1 2762.13 1 -1 2 -9 94864.1 3106.82 1 -1 2 -8 521655. 12323.9 1 -2 -1 -8 518353. 11873.3 1 2 1 -8 528461. 12357.3 1 -2 -1 -7 342029. 7883.57 1 2 1 -7 338849. 8314.27 1 -1 2 -7 341498. 8319.59 1 -2 -1 -6 204304. 4880.00 1 2 1 -6 206495. 5298.79 1 -1 2 -6 210408. 5292.55 1 2 1 -5 171135. 4428.24 1 -1 2 -5 174308. 4387.45 1 -2 -1 -5 169863. 4027.46 1 -1 2 -4 861082. 19256.2 1 2 1 -4 883714. 19321.6 1 -2 -1 -4 842222. 18889.5 1 -2 -1 -3 52551.5 1290.93 1 2 1 -3 53946.1 1627.96 1 2 1 -2 289350. 6655.26 1 1 2 1 14001.0 443.755 1 2 1 0 834669. 17677.9 2 1 2 0 790513. 17664.8 1 -1 2 1 15390.2 454.192 2 2 1 1 14160.3 535.166 2 1 2 -2 192735. 4830.84 1 2 1 2 210999. 4702.81 2 1 2 -3 56917.0 1750.90 1 1 2 -4 805206. 17985.0 1 1 2 -5 151943. 4096.34 1 -2 1 -5 157181. 3906.19 1 1 2 -6 198125. 5196.73 1 -2 1 -6 201562. 4997.23 1 1 2 -7 384395. 9390.10 1 -2 1 -7 392761. 9195.31 1 1 2 -8 528954. 12536.6 1 -2 1 -8 528933. 12342.0 1 1 2 -9 80514.7 2789.53 1 -2 1 -9 78157.6 2621.35 1 -2 1 -10 3518.43 473.162 1 1 2 -10 2780.26 479.377 1 -2 1 -11 26003.4 1384.77 1 1 2 -11 23616.9 1425.99 1 1 2 -12 139203. 4550.58 1 -2 1 -12 147286. 4415.95 1 -2 1 -13 257294. 7041.35 1 1 2 -13 255352. 7256.26 1 1 2 -14 83155.0 3364.32 1 -2 1 -14 84741.9 3189.92 1 -2 1 -15 44693.9 2203.21 1 1 2 -15 40690.5 2256.43 1 1 2 -16 68039.1 3141.23 1 -2 1 -16 69667.2 2984.05 1 -2 1 -17 16889.7 1371.45 1 1 2 -17 16522.4 1493.58 1 1 2 -18 200969. 6707.77 1 1 2 -19 202081. 6884.47 1 2 1 19 203237. 6811.07 5 2 1 20 242037. 7827.79 5 2 1 21 30327.3 2252.70 5 2 1 22 56245.6 3185.42 5 2 1 23 42789.1 2747.87 5 2 1 24 26696.9 2120.98 5 2 1 25 25046.2 2029.55 5 1 -2 25 29409.6 2204.42 5 2 1 26 5121.62 923.765 5 -2 -1 26 2870.60 684.942 5 1 -2 26 4420.42 845.514 5 1 -2 27 1483.33 437.739 5 2 1 27 2600.31 626.013 5 -2 -1 27 2679.68 617.578 5 2 1 28 14274.8 1337.68 5 -2 -1 28 16346.9 1330.49 5 1 -2 28 15223.2 1390.87 5 2 1 29 9520.10 1015.77 5 1 -2 29 10595.4 1092.24 5 2 1 30 12308.1 1055.13 5 1 -2 30 12848.3 1099.21 5 1 -2 31 -66.1865 258.312 5 2 2 0 125301. 2971.97 1 2 2 -1 181994. 4377.38 1 2 2 1 187063. 4145.00 1 2 2 -2 25646.2 961.328 1 2 2 -3 600971. 13534.4 1 2 2 -4 189835. 4811.94 1 2 2 -5 524581. 12358.1 1 -2 2 -5 545387. 12230.7 1 -2 2 -6 67671.5 2161.06 1 2 2 -6 65522.0 2247.27 1 2 2 -7 135712. 3953.29 1 -2 -2 -7 132999. 3321.37 1 -2 2 -8 182.244 180.644 1 2 2 -8 532.368 249.690 1 -2 -2 -9 265470. 6519.42 1 2 2 -9 284581. 7274.48 1 -2 2 -9 289535. 7174.81 1 -2 -2 -10 493676. 11603.5 1 2 2 -10 515945. 12411.7 1 -2 2 -10 522488. 12287.7 1 -2 2 -11 157140. 4716.75 1 2 2 -11 155879. 4848.07 1 2 2 -12 95677.5 3542.75 1 -2 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46805.6 2267.70 4 17 -6 -4 5327.25 718.262 4 17 -6 -5 3039.39 552.266 4 17 -6 -6 3486.66 574.862 4 18 0 0 189.304 279.392 4 18 0 1 7122.83 822.795 4 18 0 -1 9633.67 993.647 4 18 0 -2 -212.549 298.803 4 18 0 -3 18738.9 1392.21 4 18 0 -4 176.078 234.426 4 18 0 -5 21678.4 1475.40 4 18 0 -6 77277.7 3016.42 4 18 1 -6 28099.1 1633.22 4 18 1 -5 20423.2 1402.40 4 18 1 -4 7009.72 828.943 4 18 1 -3 2040.56 459.978 4 18 1 -2 9783.64 983.679 4 18 1 -1 1744.48 477.792 4 18 -1 1 1094.48 345.739 4 18 -1 0 20699.3 1428.56 4 18 1 0 20707.6 1445.23 4 18 1 1 3683.44 602.412 4 18 -1 -1 3445.33 586.255 4 18 -1 -2 10478.1 1037.37 4 18 -1 -3 1939.80 505.878 4 18 -1 -4 10682.2 1025.73 4 18 -1 -5 21762.7 1463.98 4 18 -1 -6 29511.5 1696.18 4 18 2 -5 42409.7 2075.96 4 18 2 -4 262.969 222.610 4 18 2 -3 4831.79 712.512 4 18 2 -2 2701.64 505.044 4 18 2 -1 15857.4 1259.99 4 18 2 0 3192.10 562.183 4 18 -2 0 4238.10 632.598 4 18 -2 -1 13618.9 1130.20 4 18 2 1 13060.2 1107.23 4 18 -2 -2 4136.44 630.002 4 18 -2 -3 5473.84 727.050 4 18 -2 -4 -310.580 244.709 4 18 -2 -5 46873.3 2213.18 4 18 3 -3 683.566 275.550 4 18 3 -2 14737.1 1179.22 4 18 3 -1 20928.7 1412.48 4 18 3 0 2296.26 477.607 4