#------------------------------------------------------------------------------ #$Date: 2017-05-20 04:58:28 +0300 (Sat, 20 May 2017) $ #$Revision: 196815 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/30/7043056.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_7043056 loop_ _publ_author_name 'Carmona, Daniel' 'Carmona, Mar\'ia' 'Rodr\'iguez, Ricardo' 'M\'endez, Isabel' 'Passarelli, Vincenzo' 'Lahoz, Fernando J.' 'Garc\'ia-Ordu\~na, Pilar' _publ_section_title ; Stereospecific control of the metal-centred chirality of rhodium(III) and iridium(III) complexes bearing tetradentate CNN’P ligands ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT01446E _journal_year 2017 _chemical_absolute_configuration rmad _chemical_formula_moiety 'C33 H30 Cl2 N2 O P Rh, 2(C H2 Cl2)' _chemical_formula_sum 'C35 H34 Cl6 N2 O P Rh' _chemical_formula_weight 845.22 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _audit_update_record ; 2017-04-21 deposited with the CCDC. 2017-05-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.9580(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.2144(7) _cell_length_b 10.5575(6) _cell_length_c 13.2353(8) _cell_measurement_reflns_used 5803 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.58 _cell_measurement_theta_min 2.351 _cell_volume 1702.67(17) _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.928 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method 'narrow \w frames' _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 0.0348 _diffrn_reflns_av_unetI/netI 0.0582 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.928 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15679 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.899 _diffrn_reflns_theta_full 26.500 _diffrn_reflns_theta_max 28.580 _diffrn_reflns_theta_min 2.470 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_T_max 0.9175 _exptl_absorpt_correction_T_min 0.7290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.649 _exptl_crystal_description needle _exptl_crystal_F_000 856 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Dichloromethane' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.050 _refine_diff_density_min -1.550 _refine_diff_density_rms 0.159 _refine_ls_abs_structure_details ; Flack x determined using 2926 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 416 _refine_ls_number_reflns 7829 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0652 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+5.5606P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1659 _refine_ls_wR_factor_ref 0.1729 _reflns_Friedel_coverage 0.840 _reflns_Friedel_fraction_full 0.994 _reflns_Friedel_fraction_max 0.866 _reflns_number_gt 7179 _reflns_number_total 7829 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01446e2.cif _cod_data_source_block cmpnd_6 _cod_database_code 7043056 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL fjl298as in P2(1) CELL 0.71073 12.2144 10.5575 13.2353 90.000 93.958 90.000 ZERR 2.00 0.0007 0.0006 0.0008 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H CL N O P RH UNIT 70 68 12 4 2 2 2 MERG 2 FMAP 2 PLAN 10 OMIT 1 0 0 OMIT 0 0 1 OMIT 3 0 0 OMIT 1 0 1 ACTA 53 BOND $H L.S. 4 TEMP -173.00 WGHT 0.086300 5.560600 FVAR 0.53716 0.70213 RH 7 0.114088 0.247833 0.146472 11.00000 0.02302 0.01665 = 0.02095 0.00025 0.00435 0.00031 CL1 3 0.183433 0.455758 0.130961 11.00000 0.03265 0.01866 = 0.02754 0.00336 0.00409 -0.00264 CL2 3 0.101054 0.225727 -0.044155 11.00000 0.04503 0.02357 = 0.02263 -0.00069 0.00491 0.00426 P 6 0.285983 0.172688 0.178970 11.00000 0.02157 0.02073 = 0.02606 0.00222 0.00635 0.00007 N1 4 0.041208 0.071047 0.161832 11.00000 0.01894 0.02122 = 0.02534 -0.00057 0.00298 -0.00213 N2 4 -0.052860 0.300772 0.129041 11.00000 0.03343 0.02140 = 0.02755 -0.00174 0.00282 -0.00157 C1 1 0.373864 0.163676 0.071561 11.00000 0.03138 0.02736 = 0.03307 -0.00303 0.00729 -0.00513 C2 1 0.365819 0.250438 -0.003884 11.00000 0.05516 0.03252 = 0.04640 0.01683 0.02246 -0.00893 AFIX 43 H2 2 0.310672 0.313896 -0.003954 11.00000 -1.20000 AFIX 0 C3 1 0.436898 0.247934 -0.080967 11.00000 0.08654 0.03912 = 0.06424 -0.00204 0.04946 -0.00196 AFIX 43 H3 2 0.432218 0.311684 -0.131739 11.00000 -1.20000 AFIX 0 C4 1 0.513032 0.155095 -0.084345 11.00000 0.04859 0.05674 = 0.06337 -0.01983 0.04106 -0.01399 AFIX 43 H4 2 0.560482 0.153254 -0.138257 11.00000 -1.20000 AFIX 0 C5 1 0.522224 0.063937 -0.010817 11.00000 0.04061 0.05841 = 0.04676 -0.02185 0.01748 -0.00132 AFIX 43 H5 2 0.575703 -0.001193 -0.012771 11.00000 -1.20000 AFIX 0 C6 1 0.451263 0.069025 0.066902 11.00000 0.03137 0.04484 = 0.04307 -0.01311 0.00873 0.00123 AFIX 43 H6 2 0.456213 0.005751 0.118049 11.00000 -1.20000 AFIX 0 C7 1 0.369599 0.257996 0.274774 11.00000 0.01885 0.03598 = 0.03683 0.01273 -0.00120 -0.00411 C8 1 0.357787 0.245096 0.377055 11.00000 0.02368 0.04825 = 0.03073 0.00709 0.00197 0.00343 AFIX 43 H8 2 0.309553 0.182392 0.400026 11.00000 -1.20000 AFIX 0 C9 1 0.415249 0.322268 0.446939 11.00000 0.04424 0.06532 = 0.03008 -0.00454 -0.00198 -0.00719 AFIX 43 H9 2 0.407637 0.309905 0.517205 11.00000 -1.20000 AFIX 0 C10 1 0.482234 0.415247 0.416346 11.00000 0.03165 0.06243 = 0.04960 -0.00935 -0.00167 -0.00671 AFIX 43 H10 2 0.520133 0.468155 0.465165 11.00000 -1.20000 AFIX 0 C11 1 0.495629 0.433397 0.313858 11.00000 0.02915 0.04451 = 0.05408 -0.00247 0.00130 -0.00966 AFIX 43 H11 2 0.542699 0.498290 0.292472 11.00000 -1.20000 AFIX 0 C12 1 0.440177 0.356637 0.243782 11.00000 0.03183 0.02969 = 0.03442 0.00069 0.00658 -0.00251 AFIX 43 H12 2 0.448865 0.369299 0.173724 11.00000 -1.20000 AFIX 0 C13 1 0.287199 0.010385 0.224898 11.00000 0.02149 0.02463 = 0.03080 0.00456 0.00820 0.00386 C14 1 0.376001 -0.036188 0.286382 11.00000 0.03205 0.02827 = 0.03950 0.00743 0.00483 0.00230 AFIX 43 H14 2 0.432505 0.019877 0.311096 11.00000 -1.20000 AFIX 0 C15 1 0.382125 -0.165337 0.311795 11.00000 0.03561 0.02895 = 0.04819 0.01442 0.00253 0.00983 AFIX 43 H15 2 0.441797 -0.195637 0.354961 11.00000 -1.20000 AFIX 0 C16 1 0.302531 -0.247939 0.274698 11.00000 0.04385 0.02574 = 0.03836 0.00299 0.01503 0.01629 AFIX 43 H16 2 0.307840 -0.335452 0.291007 11.00000 -1.20000 AFIX 0 C17 1 0.213991 -0.203191 0.213109 11.00000 0.04064 0.02390 = 0.03090 0.00238 0.01499 0.00212 AFIX 43 H17 2 0.158974 -0.260711 0.187665 11.00000 -1.20000 AFIX 0 C18 1 0.204796 -0.074360 0.188047 11.00000 0.03423 0.02000 = 0.02305 -0.00627 0.01217 0.00163 C19 1 0.105590 -0.035004 0.119882 11.00000 0.03453 0.01908 = 0.02325 -0.00175 0.00585 -0.00296 AFIX 23 H19A 2 0.130542 -0.008811 0.053422 11.00000 -1.20000 H19B 2 0.056756 -0.109207 0.108394 11.00000 -1.20000 AFIX 0 C20 1 -0.064384 0.077793 0.096218 11.00000 0.03347 0.02039 = 0.03564 -0.00205 -0.00668 0.00151 AFIX 23 H20A 2 -0.048820 0.067328 0.024271 11.00000 -1.20000 H20B 2 -0.113672 0.008204 0.114397 11.00000 -1.20000 AFIX 0 C21 1 -0.119238 0.201633 0.110159 11.00000 0.02311 0.02610 = 0.03612 0.01087 0.00025 0.00131 C22 1 -0.231555 0.216104 0.098125 11.00000 0.02292 0.02508 = 0.05990 0.01161 0.00178 -0.00066 AFIX 43 H22 2 -0.277578 0.144945 0.083582 11.00000 -1.20000 AFIX 0 C23 1 -0.277122 0.337300 0.107623 11.00000 0.02041 0.03680 = 0.05632 0.01322 0.00804 0.00550 AFIX 43 H23 2 -0.354143 0.350119 0.098345 11.00000 -1.20000 AFIX 0 C24 1 -0.206537 0.437998 0.130956 11.00000 0.03335 0.03086 = 0.03900 0.00684 0.00767 0.00916 AFIX 43 H24 2 -0.234608 0.521009 0.139150 11.00000 -1.20000 AFIX 0 C25 1 -0.096537 0.415826 0.141889 11.00000 0.03767 0.02346 = 0.02559 0.01052 0.00905 0.00817 AFIX 43 H25 2 -0.048754 0.484601 0.159323 11.00000 -1.20000 AFIX 0 C26 1 0.014191 0.046233 0.270654 11.00000 0.02557 0.02196 = 0.02498 0.00088 0.00765 -0.00413 AFIX 23 H26A 2 -0.066074 0.035432 0.273289 11.00000 -1.20000 H26B 2 0.050193 -0.033160 0.294985 11.00000 -1.20000 AFIX 0 C27 1 0.052738 0.154937 0.339272 11.00000 0.03299 0.01884 = 0.02426 0.00569 0.01107 -0.00160 C28 1 0.102442 0.259449 0.295966 11.00000 0.02350 0.02084 = 0.03077 0.00430 0.00819 -0.00023 C29 1 0.132215 0.361538 0.358858 11.00000 0.03603 0.02262 = 0.02647 -0.00170 0.00810 0.00027 AFIX 43 H29 2 0.165058 0.434162 0.331255 11.00000 -1.20000 AFIX 0 C30 1 0.114412 0.358337 0.461517 11.00000 0.05134 0.01927 = 0.02625 0.00162 0.00572 0.00295 AFIX 43 H30 2 0.138285 0.426682 0.504231 11.00000 -1.20000 AFIX 0 C31 1 0.061448 0.254621 0.501692 11.00000 0.06192 0.02655 = 0.02390 -0.00407 0.01623 -0.00154 C32 1 0.032530 0.149951 0.441564 11.00000 0.05257 0.01837 = 0.03538 0.00112 0.02465 -0.00445 AFIX 43 H32 2 -0.000004 0.077314 0.469453 11.00000 -1.20000 AFIX 0 C33 1 -0.001286 0.154707 0.648725 11.00000 0.08860 0.03493 = 0.04280 0.00484 0.03705 0.00630 AFIX 137 H33A 2 -0.078455 0.148241 0.623603 11.00000 -1.50000 H33B 2 0.003372 0.163392 0.722617 11.00000 -1.50000 H33C 2 0.038013 0.078202 0.630032 11.00000 -1.50000 AFIX 0 O 5 0.047761 0.264414 0.604308 11.00000 0.10673 0.02728 = 0.02511 0.00309 0.02955 0.00222 C51 1 0.234505 0.318054 0.745313 11.00000 0.06801 0.08322 = 0.06722 0.01442 0.00591 -0.01523 AFIX 23 H51A 2 0.158789 0.332509 0.715938 11.00000 -1.20000 H51B 2 0.230940 0.294734 0.817461 11.00000 -1.20000 AFIX 0 CL3 3 0.299683 0.189045 0.676349 11.00000 0.09772 0.08496 = 0.09567 0.00309 0.01542 0.01954 CL4 3 0.313026 0.456231 0.735037 11.00000 0.09463 0.08025 = 0.11481 0.01486 0.00910 0.00678 C52 1 0.237298 0.781531 0.604415 11.00000 0.05502 0.10012 = 0.09613 0.01875 0.00885 -0.01766 part 1 AFIX 23 H52A 2 0.169976 0.755391 0.636440 21.00000 -1.20000 H52B 2 0.293608 0.805210 0.658506 21.00000 -1.20000 AFIX 23 part 2 H52C 2 0.277903 0.822222 0.663072 -21.00000 -1.20000 H52D 2 0.164027 0.762180 0.628143 -21.00000 -1.20000 AFIX 0 part 0 CL5 3 0.209287 0.909445 0.523744 11.00000 0.06988 0.09092 = 0.09586 -0.00751 0.02684 -0.00670 PART 1 CL6A 3 0.285230 0.657039 0.531592 21.00000 0.07471 PART 2 CL6B 3 0.294282 0.641173 0.603055 -21.00000 0.12664 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl298as in P2(1) REM R1 = 0.0652 for 7179 Fo > 4sig(Fo) and 0.0722 for all 7829 data REM 416 parameters refined using 1 restraints END WGHT 0.0839 5.8769 REM Highest difference peak 1.050, deepest hole -1.550, 1-sigma level 0.159 Q1 1 0.0486 0.2449 0.1162 11.00000 0.05 1.05 Q2 1 0.2382 0.6696 0.5184 11.00000 0.05 0.88 Q3 1 0.3333 0.6391 0.5402 11.00000 0.05 0.85 Q4 1 0.1826 0.2537 0.1790 11.00000 0.05 0.70 Q5 1 0.2434 0.8303 0.5149 11.00000 0.05 0.68 Q6 1 0.2508 0.9955 0.5831 11.00000 0.05 0.64 Q7 1 0.3339 0.8613 0.5359 11.00000 0.05 0.63 Q8 1 0.3995 0.2568 -0.1305 11.00000 0.05 0.56 Q9 1 0.1154 0.2525 0.6197 11.00000 0.05 0.56 Q10 1 0.2840 0.5919 0.6611 11.00000 0.05 0.55 ; _shelx_res_checksum 61014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.11409(5) 0.24783(6) 0.14647(5) 0.02008(17) Uani 1 1 d . . . . . Cl1 Cl 0.1834(2) 0.4558(2) 0.13096(18) 0.0262(5) Uani 1 1 d . . . . . Cl2 Cl 0.1011(2) 0.2257(2) -0.04416(17) 0.0303(6) Uani 1 1 d . . . . . P P 0.2860(2) 0.1727(2) 0.17897(19) 0.0226(5) Uani 1 1 d . . . . . N1 N 0.0412(7) 0.0710(8) 0.1618(6) 0.0218(16) Uani 1 1 d . . . . . N2 N -0.0529(8) 0.3008(9) 0.1290(7) 0.0274(18) Uani 1 1 d . . . . . C1 C 0.3739(9) 0.1637(11) 0.0716(8) 0.030(2) Uani 1 1 d . . . . . C2 C 0.3658(10) 0.2504(16) -0.0039(9) 0.044(3) Uani 1 1 d . . . . . H2 H 0.3107 0.3139 -0.0040 0.053 Uiso 1 1 calc R U . . . C3 C 0.4369(13) 0.2479(19) -0.0810(11) 0.061(4) Uani 1 1 d . . . . . H3 H 0.4322 0.3117 -0.1317 0.074 Uiso 1 1 calc R U . . . C4 C 0.5130(12) 0.1551(15) -0.0843(12) 0.055(4) Uani 1 1 d . . . . . H4 H 0.5605 0.1533 -0.1383 0.065 Uiso 1 1 calc R U . . . C5 C 0.5222(11) 0.0639(15) -0.0108(10) 0.048(3) Uani 1 1 d . . . . . H5 H 0.5757 -0.0012 -0.0128 0.058 Uiso 1 1 calc R U . . . C6 C 0.4513(10) 0.0690(13) 0.0669(10) 0.039(3) Uani 1 1 d . . . . . H6 H 0.4562 0.0058 0.1180 0.047 Uiso 1 1 calc R U . . . C7 C 0.3696(7) 0.2580(14) 0.2748(8) 0.031(2) Uani 1 1 d . . . . . C8 C 0.3578(8) 0.2451(17) 0.3771(7) 0.034(2) Uani 1 1 d . . . . . H8 H 0.3096 0.1824 0.4000 0.041 Uiso 1 1 calc R U . . . C9 C 0.4152(11) 0.3223(15) 0.4469(10) 0.047(3) Uani 1 1 d . . . . . H9 H 0.4076 0.3099 0.5172 0.056 Uiso 1 1 calc R U . . . C10 C 0.4822(11) 0.4152(15) 0.4163(11) 0.048(3) Uani 1 1 d . . . . . H10 H 0.5201 0.4682 0.4652 0.058 Uiso 1 1 calc R U . . . C11 C 0.4956(10) 0.4334(13) 0.3139(10) 0.043(3) Uani 1 1 d . . . . . H11 H 0.5427 0.4983 0.2925 0.051 Uiso 1 1 calc R U . . . C12 C 0.4402(9) 0.3566(11) 0.2438(9) 0.032(2) Uani 1 1 d . . . . . H12 H 0.4489 0.3693 0.1737 0.038 Uiso 1 1 calc R U . . . C13 C 0.2872(8) 0.0104(10) 0.2249(8) 0.025(2) Uani 1 1 d . . . . . C14 C 0.3760(9) -0.0362(11) 0.2864(9) 0.033(2) Uani 1 1 d . . . . . H14 H 0.4325 0.0199 0.3111 0.040 Uiso 1 1 calc R U . . . C15 C 0.3821(10) -0.1653(11) 0.3118(10) 0.038(3) Uani 1 1 d . . . . . H15 H 0.4418 -0.1956 0.3550 0.045 Uiso 1 1 calc R U . . . C16 C 0.3025(9) -0.2479(15) 0.2747(8) 0.035(2) Uani 1 1 d . . . . . H16 H 0.3078 -0.3355 0.2910 0.043 Uiso 1 1 calc R U . . . C17 C 0.2140(10) -0.2032(10) 0.2131(8) 0.031(2) Uani 1 1 d . . . . . H17 H 0.1590 -0.2607 0.1877 0.037 Uiso 1 1 calc R U . . . C18 C 0.2048(9) -0.0744(9) 0.1880(7) 0.025(2) Uani 1 1 d . . . . . C19 C 0.1056(9) -0.0350(9) 0.1199(7) 0.025(2) Uani 1 1 d . . . . . H19A H 0.1305 -0.0088 0.0534 0.031 Uiso 1 1 calc R U . . . H19B H 0.0568 -0.1092 0.1084 0.031 Uiso 1 1 calc R U . . . C20 C -0.0644(9) 0.0778(10) 0.0962(9) 0.030(2) Uani 1 1 d . . . . . H20A H -0.0488 0.0673 0.0243 0.036 Uiso 1 1 calc R U . . . H20B H -0.1137 0.0082 0.1144 0.036 Uiso 1 1 calc R U . . . C21 C -0.1192(9) 0.2016(10) 0.1102(8) 0.029(2) Uani 1 1 d . . . . . C22 C -0.2316(9) 0.2161(10) 0.0981(10) 0.036(3) Uani 1 1 d . . . . . H22 H -0.2776 0.1449 0.0836 0.043 Uiso 1 1 calc R U . . . C23 C -0.2771(9) 0.3373(12) 0.1076(10) 0.038(3) Uani 1 1 d . . . . . H23 H -0.3541 0.3501 0.0983 0.045 Uiso 1 1 calc R U . . . C24 C -0.2065(9) 0.4380(11) 0.1310(9) 0.034(2) Uani 1 1 d . . . . . H24 H -0.2346 0.5210 0.1392 0.041 Uiso 1 1 calc R U . . . C25 C -0.0965(9) 0.4158(10) 0.1419(8) 0.029(2) Uani 1 1 d . . . . . H25 H -0.0488 0.4846 0.1593 0.034 Uiso 1 1 calc R U . . . C26 C 0.0142(8) 0.0462(9) 0.2707(7) 0.0239(19) Uani 1 1 d . . . . . H26A H -0.0661 0.0354 0.2733 0.029 Uiso 1 1 calc R U . . . H26B H 0.0502 -0.0332 0.2950 0.029 Uiso 1 1 calc R U . . . C27 C 0.0527(9) 0.1549(9) 0.3393(8) 0.025(2) Uani 1 1 d . . . . . C28 C 0.1024(7) 0.2594(12) 0.2960(7) 0.0247(19) Uani 1 1 d . . . . . C29 C 0.1322(9) 0.3615(10) 0.3589(8) 0.028(2) Uani 1 1 d . . . . . H29 H 0.1651 0.4342 0.3313 0.034 Uiso 1 1 calc R U . . . C30 C 0.1144(10) 0.3583(10) 0.4615(8) 0.032(2) Uani 1 1 d . . . . . H30 H 0.1383 0.4267 0.5042 0.039 Uiso 1 1 calc R U . . . C31 C 0.0614(10) 0.2546(14) 0.5017(7) 0.037(2) Uani 1 1 d . . . . . C32 C 0.0325(11) 0.1500(10) 0.4416(9) 0.034(3) Uani 1 1 d . . . . . H32 H 0.0000 0.0773 0.4695 0.041 Uiso 1 1 calc R U . . . C33 C -0.0013(14) 0.1547(13) 0.6487(10) 0.054(4) Uani 1 1 d . . . . . H33A H -0.0785 0.1482 0.6236 0.081 Uiso 1 1 calc R U . . . H33B H 0.0034 0.1634 0.7226 0.081 Uiso 1 1 calc R U . . . H33C H 0.0380 0.0782 0.6300 0.081 Uiso 1 1 calc R U . . . O O 0.0478(9) 0.2644(9) 0.6043(6) 0.052(3) Uani 1 1 d . . . . . C51 C 0.2345(16) 0.318(2) 0.7453(15) 0.073(5) Uani 1 1 d . . . . . H51A H 0.1588 0.3325 0.7159 0.087 Uiso 1 1 calc R U . . . H51B H 0.2309 0.2947 0.8175 0.087 Uiso 1 1 calc R U . . . Cl3 Cl 0.2997(5) 0.1890(6) 0.6763(5) 0.0924(16) Uani 1 1 d . . . . . Cl4 Cl 0.3130(5) 0.4562(6) 0.7350(5) 0.0965(17) Uani 1 1 d . . . . . C52 C 0.2373(15) 0.782(2) 0.6044(17) 0.084(7) Uani 1 1 d . . . . . H52A H 0.1700 0.7554 0.6364 0.100 Uiso 0.70(2) 1 calc R U P A 1 H52B H 0.2936 0.8052 0.6585 0.100 Uiso 0.70(2) 1 calc R U P A 1 H52C H 0.2779 0.8222 0.6631 0.100 Uiso 0.30(2) 1 calc R U P A 2 H52D H 0.1640 0.7622 0.6281 0.100 Uiso 0.30(2) 1 calc R U P A 2 Cl5 Cl 0.2093(4) 0.9094(6) 0.5237(5) 0.0846(15) Uani 1 1 d . . . . . Cl6A Cl 0.2852(6) 0.6570(7) 0.5316(7) 0.075(3) Uiso 0.70(2) 1 d . . P A 1 Cl6B Cl 0.294(2) 0.641(3) 0.603(3) 0.127(12) Uiso 0.30(2) 1 d . . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.0230(3) 0.0167(3) 0.0210(3) 0.0002(3) 0.0044(2) 0.0003(3) Cl1 0.0327(12) 0.0187(10) 0.0275(11) 0.0034(9) 0.0041(9) -0.0026(9) Cl2 0.0450(13) 0.0236(15) 0.0226(10) -0.0007(8) 0.0049(9) 0.0043(10) P 0.0216(12) 0.0207(12) 0.0261(12) 0.0022(9) 0.0063(9) 0.0001(9) N1 0.019(4) 0.021(4) 0.025(4) -0.001(3) 0.003(3) -0.002(3) N2 0.033(5) 0.021(4) 0.028(4) -0.002(3) 0.003(4) -0.002(4) C1 0.031(5) 0.027(5) 0.033(5) -0.003(4) 0.007(4) -0.005(4) C2 0.055(6) 0.033(5) 0.046(6) 0.017(7) 0.022(5) -0.009(8) C3 0.087(10) 0.039(6) 0.064(8) -0.002(10) 0.049(7) -0.002(10) C4 0.049(8) 0.057(9) 0.063(9) -0.020(7) 0.041(7) -0.014(7) C5 0.041(7) 0.058(9) 0.047(7) -0.022(7) 0.017(6) -0.001(6) C6 0.031(6) 0.045(7) 0.043(6) -0.013(5) 0.009(5) 0.001(5) C7 0.019(4) 0.036(6) 0.037(5) 0.013(6) -0.001(3) -0.004(5) C8 0.024(4) 0.048(6) 0.031(4) 0.007(7) 0.002(3) 0.003(7) C9 0.044(7) 0.065(9) 0.030(6) -0.005(6) -0.002(5) -0.007(7) C10 0.032(6) 0.062(9) 0.050(7) -0.009(7) -0.002(5) -0.007(6) C11 0.029(6) 0.045(7) 0.054(8) -0.002(6) 0.001(5) -0.010(5) C12 0.032(5) 0.030(5) 0.034(5) 0.001(4) 0.007(4) -0.003(4) C13 0.021(5) 0.025(5) 0.031(5) 0.005(4) 0.008(4) 0.004(4) C14 0.032(6) 0.028(5) 0.040(6) 0.007(5) 0.005(5) 0.002(4) C15 0.036(6) 0.029(6) 0.048(7) 0.014(5) 0.003(5) 0.010(5) C16 0.044(5) 0.026(5) 0.038(5) 0.003(6) 0.015(4) 0.016(6) C17 0.041(6) 0.024(5) 0.031(5) 0.002(4) 0.015(5) 0.002(4) C18 0.034(5) 0.020(5) 0.023(4) -0.006(3) 0.012(4) 0.002(4) C19 0.035(5) 0.019(4) 0.023(4) -0.002(4) 0.006(4) -0.003(4) C20 0.033(6) 0.020(5) 0.036(6) -0.002(4) -0.007(5) 0.002(4) C21 0.023(5) 0.026(5) 0.036(5) 0.011(4) 0.000(4) 0.001(4) C22 0.023(5) 0.025(6) 0.060(7) 0.012(5) 0.002(5) -0.001(4) C23 0.020(5) 0.037(6) 0.056(7) 0.013(5) 0.008(5) 0.005(5) C24 0.033(6) 0.031(6) 0.039(6) 0.007(5) 0.008(5) 0.009(5) C25 0.038(6) 0.023(5) 0.026(5) 0.011(4) 0.009(4) 0.008(4) C26 0.026(5) 0.022(4) 0.025(4) 0.001(4) 0.008(4) -0.004(4) C27 0.033(5) 0.019(4) 0.024(5) 0.006(4) 0.011(4) -0.002(4) C28 0.023(4) 0.021(5) 0.031(4) 0.004(5) 0.008(3) 0.000(4) C29 0.036(6) 0.023(5) 0.026(5) -0.002(4) 0.008(4) 0.000(4) C30 0.051(7) 0.019(5) 0.026(5) 0.002(4) 0.006(5) 0.003(4) C31 0.062(7) 0.027(5) 0.024(4) -0.004(5) 0.016(4) -0.002(7) C32 0.053(7) 0.018(5) 0.035(6) 0.001(4) 0.025(5) -0.004(5) C33 0.089(11) 0.035(7) 0.043(7) 0.005(6) 0.037(7) 0.006(7) O 0.107(8) 0.027(5) 0.025(3) 0.003(4) 0.030(4) 0.002(5) C51 0.068(11) 0.083(13) 0.067(11) 0.014(10) 0.006(9) -0.015(10) Cl3 0.098(4) 0.085(4) 0.096(4) 0.003(3) 0.015(3) 0.020(3) Cl4 0.095(4) 0.080(4) 0.115(4) 0.015(3) 0.009(3) 0.007(3) C52 0.055(10) 0.100(19) 0.096(14) 0.019(12) 0.009(9) -0.018(10) Cl5 0.070(3) 0.091(4) 0.096(4) -0.008(3) 0.027(3) -0.007(3) 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' P P 0.1023 0.0942 '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 C28 Rh N1 84.2(4) C28 Rh N2 87.6(4) N1 Rh N2 80.3(3) C28 Rh P 87.8(3) N1 Rh P 93.7(2) N2 Rh P 172.8(3) C28 Rh Cl1 94.6(3) N1 Rh Cl1 175.5(2) N2 Rh Cl1 95.4(3) P Rh Cl1 90.50(9) C28 Rh Cl2 172.1(3) N1 Rh Cl2 91.0(2) N2 Rh Cl2 85.5(2) P Rh Cl2 98.71(9) Cl1 Rh Cl2 89.85(8) C7 P C13 104.1(5) C7 P C1 103.6(5) C13 P C1 102.6(5) C7 P Rh 115.5(4) C13 P Rh 112.4(3) C1 P Rh 117.1(4) C19 N1 C20 105.8(8) C19 N1 C26 112.1(7) C20 N1 C26 108.7(8) C19 N1 Rh 113.3(6) C20 N1 Rh 104.8(6) C26 N1 Rh 111.6(6) C21 N2 C25 119.4(10) C21 N2 Rh 112.4(7) C25 N2 Rh 128.0(8) C2 C1 C6 118.2(11) C2 C1 P 121.2(9) C6 C1 P 120.6(9) C1 C2 C3 120.9(15) C1 C2 H2 119.6 C3 C2 H2 119.6 C4 C3 C2 120.3(16) C4 C3 H3 119.8 C2 C3 H3 119.8 C3 C4 C5 120.6(12) C3 C4 H4 119.7 C5 C4 H4 119.7 C4 C5 C6 118.3(13) C4 C5 H5 120.8 C6 C5 H5 120.8 C1 C6 C5 121.7(13) C1 C6 H6 119.2 C5 C6 H6 119.2 C8 C7 C12 117.4(12) C8 C7 P 123.1(9) C12 C7 P 118.9(8) C7 C8 C9 121.0(13) C7 C8 H8 119.5 C9 C8 H8 119.5 C10 C9 C8 120.9(12) C10 C9 H9 119.5 C8 C9 H9 119.5 C9 C10 C11 120.3(13) C9 C10 H10 119.9 C11 C10 H10 119.9 C12 C11 C10 119.4(12) C12 C11 H11 120.3 C10 C11 H11 120.3 C11 C12 C7 121.0(11) C11 C12 H12 119.5 C7 C12 H12 119.5 C14 C13 C18 119.0(10) C14 C13 P 120.9(8) C18 C13 P 119.6(8) C13 C14 C15 120.4(11) C13 C14 H14 119.8 C15 C14 H14 119.8 C16 C15 C14 120.4(11) C16 C15 H15 119.8 C14 C15 H15 119.8 C15 C16 C17 119.8(13) C15 C16 H16 120.1 C17 C16 H16 120.1 C16 C17 C18 120.9(12) C16 C17 H17 119.5 C18 C17 H17 119.5 C17 C18 C13 119.4(10) C17 C18 C19 117.0(10) C13 C18 C19 123.6(9) N1 C19 C18 113.7(8) N1 C19 H19A 108.8 C18 C19 H19A 108.8 N1 C19 H19B 108.8 C18 C19 H19B 108.8 H19A C19 H19B 107.7 C21 C20 N1 110.2(9) C21 C20 H20A 109.6 N1 C20 H20A 109.6 C21 C20 H20B 109.6 N1 C20 H20B 109.6 H20A C20 H20B 108.1 N2 C21 C22 121.4(10) N2 C21 C20 116.0(9) C22 C21 C20 122.5(10) C21 C22 C23 119.2(10) C21 C22 H22 120.4 C23 C22 H22 120.4 C24 C23 C22 118.2(10) C24 C23 H23 120.9 C22 C23 H23 120.9 C25 C24 C23 119.0(11) C25 C24 H24 120.5 C23 C24 H24 120.5 N2 C25 C24 122.7(11) N2 C25 H25 118.7 C24 C25 H25 118.7 C27 C26 N1 110.9(7) C27 C26 H26A 109.5 N1 C26 H26A 109.5 C27 C26 H26B 109.5 N1 C26 H26B 109.5 H26A C26 H26B 108.0 C32 C27 C28 122.5(10) C32 C27 C26 119.0(9) C28 C27 C26 118.4(9) C29 C28 C27 117.8(9) C29 C28 Rh 127.2(8) C27 C28 Rh 114.8(8) C30 C29 C28 120.8(10) C30 C29 H29 119.6 C28 C29 H29 119.6 C29 C30 C31 119.9(10) C29 C30 H30 120.0 C31 C30 H30 120.0 O C31 C32 125.2(11) O C31 C30 114.0(11) C32 C31 C30 120.7(9) C31 C32 C27 118.0(9) C31 C32 H32 121.0 C27 C32 H32 121.0 O C33 H33A 109.5 O C33 H33B 109.5 H33A C33 H33B 109.5 O C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C31 O C33 114.9(11) Cl4 C51 Cl3 108.5(10) Cl4 C51 H51A 110.0 Cl3 C51 H51A 110.0 Cl4 C51 H51B 110.0 Cl3 C51 H51B 110.0 H51A C51 H51B 108.4 Cl6B C52 Cl5 140(2) Cl5 C52 Cl6A 107.6(12) Cl5 C52 H52A 110.2 Cl6A C52 H52A 110.2 Cl5 C52 H52B 110.2 Cl6A C52 H52B 110.2 H52A C52 H52B 108.5 Cl6B C52 H52C 102.2 Cl5 C52 H52C 102.2 Cl6B C52 H52D 102.2 Cl5 C52 H52D 102.2 H52C C52 H52D 104.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Rh C28 1.997(9) Rh N1 2.084(8) Rh N2 2.112(10) Rh P 2.258(3) Rh Cl1 2.367(2) Rh Cl2 2.528(2) P C7 1.812(12) P C13 1.818(10) P C1 1.842(11) N1 C19 1.497(13) N1 C20 1.506(13) N1 C26 1.522(12) N2 C21 1.337(14) N2 C25 1.342(13) C1 C2 1.354(17) C1 C6 1.380(17) C2 C3 1.385(15) C2 H2 0.9500 C3 C4 1.35(2) C3 H3 0.9500 C4 C5 1.37(2) C4 H4 0.9500 C5 C6 1.391(16) C5 H5 0.9500 C6 H6 0.9500 C7 C8 1.378(13) C7 C12 1.430(15) C8 C9 1.386(18) C8 H8 0.9500 C9 C10 1.36(2) C9 H9 0.9500 C10 C11 1.39(2) C10 H10 0.9500 C11 C12 1.374(17) C11 H11 0.9500 C12 H12 0.9500 C13 C14 1.400(15) C13 C18 1.408(15) C14 C15 1.405(16) C14 H14 0.9500 C15 C16 1.371(19) C15 H15 0.9500 C16 C17 1.391(16) C16 H16 0.9500 C17 C18 1.403(14) C17 H17 0.9500 C18 C19 1.518(15) C19 H19A 0.9900 C19 H19B 0.9900 C20 C21 1.486(15) C20 H20A 0.9900 C20 H20B 0.9900 C21 C22 1.379(15) C22 C23 1.404(16) C22 H22 0.9500 C23 C24 1.390(18) C23 H23 0.9500 C24 C25 1.362(16) C24 H24 0.9500 C25 H25 0.9500 C26 C27 1.518(14) C26 H26A 0.9900 C26 H26B 0.9900 C27 C32 1.394(14) C27 C28 1.401(14) C28 C29 1.395(15) C29 C30 1.391(14) C29 H29 0.9500 C30 C31 1.396(17) C30 H30 0.9500 C31 O 1.384(11) C31 C32 1.393(17) C32 H32 0.9500 C33 O 1.447(16) C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C51 Cl4 1.76(2) C51 Cl3 1.85(2) C51 H51A 0.9900 C51 H51B 0.9900 C52 Cl6B 1.64(4) C52 Cl5 1.74(2) C52 Cl6A 1.75(2) C52 H52A 0.9900 C52 H52B 0.9900 C52 H52C 0.9900 C52 H52D 0.9900