#------------------------------------------------------------------------------ #$Date: 2017-05-20 04:58:28 +0300 (Sat, 20 May 2017) $ #$Revision: 196815 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/30/7043055.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_7043055 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_formula_moiety 'C33 H27 Cl2 F3 N2 P Rh, 0.5(H2 O)' _chemical_formula_sum 'C33 H28 Cl2 F3 N2 O0.5 P Rh' _chemical_formula_weight 722.35 _chemical_name_systematic ; ? ; _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3199(6) _cell_length_b 11.3820(5) _cell_length_c 20.6691(9) _cell_measurement_reflns_used 9923 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.493 _cell_measurement_theta_min 2.353 _cell_volume 3133.6(2) _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 0.998 _diffrn_measured_fraction_theta_max 0.940 _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 0.0215 _diffrn_reflns_av_unetI/netI 0.0169 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 36228 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.919 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.625 _diffrn_reflns_theta_min 1.971 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_T_max 0.8422 _exptl_absorpt_correction_T_min 0.7663 _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 1.531 _exptl_crystal_description prism _exptl_crystal_F_000 1460 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Dichloromethane' _exptl_crystal_size_max 0.392 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.834 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.067 _refine_ls_abs_structure_details ; Flack x determined using 3341 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.030(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 7377 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.974 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0207 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.6560P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.0563 _reflns_Friedel_coverage 0.901 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.896 _reflns_number_gt 7187 _reflns_number_total 7377 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01446e2.cif _cod_data_source_block cmpnd_7 _cod_original_formula_sum 'C33 H28 Cl2 F3 N2 O0.50 P Rh' _cod_database_code 7043055 _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 fjl325as in Pca2(1) CELL 0.71073 13.3199 11.3820 20.6691 90.000 90.000 90.000 ZERR 4.00 0.0006 0.0005 0.0009 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, Y, 1/2 + Z SYMM 1/2 + X, - Y, Z SFAC C H CL F N P RH O UNIT 132 112 8 12 8 4 4 2 MERG 2 FMAP 2 PLAN 15 OMIT 0 0 -2 OMIT 0 1 0 OMIT 0 1 2 OMIT 1 5 0 TEMP -173 ACTA BOND $H CONF L.S. 4 SUMP 0.5 0.01 1.0 2 1.0 3 WGHT 0.042200 0.656000 FVAR 0.10478 0.31170 0.18119 0.08556 RH 7 0.636028 0.652554 0.516799 11.00000 0.01304 0.01201 = 0.01363 -0.00004 -0.00089 0.00053 CL1 3 0.789744 0.725456 0.557165 11.00000 0.01512 0.02322 = 0.02244 -0.00306 -0.00274 -0.00076 CL2 3 0.721957 0.502020 0.450079 11.00000 0.01761 0.01666 = 0.02258 -0.00194 0.00071 0.00416 P 6 0.635232 0.786875 0.436144 11.00000 0.01552 0.01217 = 0.01572 0.00026 0.00019 -0.00059 F1 4 0.373881 1.080803 0.682897 11.00000 0.06893 0.02466 = 0.05037 -0.00387 0.02681 0.01503 F2 4 0.369589 0.943447 0.752807 11.00000 0.04061 0.04272 = 0.01886 -0.00687 0.00520 0.00449 F3 4 0.258555 0.948091 0.677905 11.00000 0.02700 0.06860 = 0.04501 -0.02704 -0.00263 0.01781 N1 5 0.497123 0.579522 0.492994 11.00000 0.01403 0.01167 = 0.01559 0.00120 -0.00025 -0.00005 N2 5 0.624461 0.525992 0.591286 11.00000 0.01917 0.01964 = 0.01884 0.00203 -0.00148 -0.00023 C1 1 0.731879 0.767243 0.374321 11.00000 0.02330 0.01380 = 0.02064 0.00100 0.00450 -0.00109 C2 1 0.710543 0.777071 0.308295 11.00000 0.02899 0.02248 = 0.02038 0.00229 0.00129 0.00430 AFIX 43 H2 2 0.643562 0.791399 0.294617 11.00000 -1.20000 AFIX 0 C3 1 0.786322 0.766090 0.262500 11.00000 0.04074 0.03007 = 0.02240 0.00611 0.00913 0.01057 AFIX 43 H3 2 0.770871 0.772011 0.217748 11.00000 -1.20000 AFIX 0 C4 1 0.884319 0.746528 0.282027 11.00000 0.03569 0.03221 = 0.03112 0.00851 0.01692 0.00769 AFIX 43 H4 2 0.936259 0.740676 0.250693 11.00000 -1.20000 AFIX 0 C5 1 0.906826 0.735445 0.347357 11.00000 0.02420 0.03129 = 0.03743 0.00456 0.00815 0.00512 AFIX 43 H5 2 0.973987 0.721203 0.360690 11.00000 -1.20000 AFIX 0 C6 1 0.831017 0.745214 0.393143 11.00000 0.02406 0.02703 = 0.02308 0.00435 0.00255 0.00357 AFIX 43 H6 2 0.846628 0.736847 0.437754 11.00000 -1.20000 AFIX 0 C7 1 0.648847 0.939852 0.460892 11.00000 0.02167 0.01271 = 0.01748 0.00274 -0.00143 -0.00127 C8 1 0.566646 1.001791 0.485438 11.00000 0.02395 0.01832 = 0.02207 -0.00031 -0.00076 0.00049 AFIX 43 H8 2 0.503638 0.963495 0.489802 11.00000 -1.20000 AFIX 0 C9 1 0.576127 1.118212 0.503425 11.00000 0.03084 0.01979 = 0.02688 -0.00408 -0.00395 0.00543 AFIX 43 H9 2 0.519507 1.159737 0.519496 11.00000 -1.20000 AFIX 0 C10 1 0.668280 1.174733 0.498069 11.00000 0.03796 0.01546 = 0.03146 -0.00164 -0.00606 -0.00342 AFIX 43 H10 2 0.674763 1.255059 0.509836 11.00000 -1.20000 AFIX 0 C11 1 0.750561 1.112693 0.475392 11.00000 0.02877 0.02083 = 0.02932 0.00043 -0.00240 -0.00751 AFIX 43 H11 2 0.813946 1.150586 0.472456 11.00000 -1.20000 AFIX 0 C12 1 0.741638 0.995952 0.456909 11.00000 0.02444 0.01803 = 0.02216 0.00128 0.00034 -0.00294 AFIX 43 H12 2 0.798695 0.954340 0.441564 11.00000 -1.20000 AFIX 0 C13 1 0.516876 0.789413 0.391685 11.00000 0.01981 0.01568 = 0.01506 0.00011 -0.00189 0.00170 C14 1 0.489413 0.891584 0.357248 11.00000 0.02562 0.01551 = 0.01785 0.00322 0.00023 -0.00060 AFIX 43 H14 2 0.532985 0.957661 0.357508 11.00000 -1.20000 AFIX 0 C15 1 0.400103 0.897224 0.323094 11.00000 0.02630 0.01970 = 0.02066 0.00384 -0.00006 0.00525 AFIX 43 H15 2 0.383002 0.966346 0.299809 11.00000 -1.20000 AFIX 0 C16 1 0.335462 0.800995 0.323062 11.00000 0.02103 0.02554 = 0.01968 0.00187 -0.00389 0.00395 AFIX 43 H16 2 0.273594 0.804457 0.300274 11.00000 -1.20000 AFIX 0 C17 1 0.362243 0.699596 0.356714 11.00000 0.02030 0.02176 = 0.01491 -0.00076 0.00052 -0.00225 AFIX 43 H17 2 0.318022 0.634112 0.356439 11.00000 -1.20000 AFIX 0 C18 1 0.452042 0.691987 0.390649 11.00000 0.01996 0.01577 = 0.01176 -0.00036 0.00069 0.00066 C19 1 0.476629 0.575693 0.421794 11.00000 0.01937 0.01332 = 0.01357 -0.00022 -0.00157 -0.00057 AFIX 23 H19A 2 0.419882 0.521278 0.414117 11.00000 -1.20000 H19B 2 0.536260 0.542385 0.399861 11.00000 -1.20000 AFIX 0 C20 1 0.503469 0.453632 0.514576 11.00000 0.02178 0.01192 = 0.01783 0.00246 -0.00216 -0.00074 AFIX 23 H20A 2 0.435230 0.419288 0.516205 11.00000 -1.20000 H20B 2 0.543582 0.408016 0.483033 11.00000 -1.20000 AFIX 0 C21 1 0.551082 0.445753 0.579975 11.00000 0.02075 0.01680 = 0.02106 0.00262 -0.00283 -0.00019 C22 1 0.527065 0.360708 0.625114 11.00000 0.03553 0.02488 = 0.03072 0.00974 -0.00821 -0.00812 AFIX 43 H22 2 0.475249 0.305412 0.616726 11.00000 -1.20000 AFIX 0 C23 1 0.580116 0.357530 0.683040 11.00000 0.05810 0.04460 = 0.03321 0.02391 -0.01658 -0.01873 AFIX 43 H23 2 0.565536 0.299433 0.714673 11.00000 -1.20000 AFIX 0 C24 1 0.653846 0.439491 0.693891 11.00000 0.05948 0.04737 = 0.02993 0.01635 -0.02300 -0.01579 AFIX 43 H24 2 0.690541 0.438918 0.733302 11.00000 -1.20000 AFIX 0 C25 1 0.674426 0.523283 0.646834 11.00000 0.03619 0.02956 = 0.02564 0.00653 -0.00942 -0.00653 AFIX 43 H25 2 0.725413 0.579919 0.654592 11.00000 -1.20000 AFIX 0 C26 1 0.413110 0.639844 0.529992 11.00000 0.01584 0.01680 = 0.01659 -0.00002 0.00172 0.00040 AFIX 23 H26A 2 0.363943 0.672593 0.498927 11.00000 -1.20000 H26B 2 0.377901 0.581327 0.557213 11.00000 -1.20000 AFIX 0 C27 1 0.452550 0.736797 0.572106 11.00000 0.02006 0.01616 = 0.01461 0.00058 -0.00134 0.00094 C28 1 0.555209 0.760608 0.571984 11.00000 0.01879 0.01496 = 0.01332 0.00029 -0.00178 0.00058 C29 1 0.591270 0.852755 0.610883 11.00000 0.01908 0.02120 = 0.01796 -0.00335 -0.00213 0.00009 AFIX 43 H29 2 0.661051 0.869985 0.611412 11.00000 -1.20000 AFIX 0 C30 1 0.526289 0.918489 0.648338 11.00000 0.02831 0.01921 = 0.01588 -0.00482 -0.00271 0.00057 AFIX 43 H30 2 0.551571 0.980585 0.674373 11.00000 -1.20000 AFIX 0 C31 1 0.423920 0.894062 0.648064 11.00000 0.02665 0.02184 = 0.01504 -0.00175 0.00061 0.00623 C32 1 0.386307 0.802070 0.610066 11.00000 0.01904 0.02647 = 0.01687 -0.00211 0.00034 0.00461 AFIX 43 H32 2 0.316603 0.784392 0.610158 11.00000 -1.20000 AFIX 0 C33 1 0.356555 0.965673 0.689557 11.00000 0.03004 0.03002 = 0.02227 -0.00817 0.00330 0.00611 part 1 O1A 8 0.671083 0.477109 0.304082 21.00000 41.00000 part 2 O1B 8 0.592695 0.475607 0.273392 31.00000 41.00000 part 0 HKLF 4 REM fjl325as in Pca2(1) REM R1 = 0.0207 for 7187 Fo > 4sig(Fo) and 0.0216 for all 7377 data REM 388 parameters refined using 2 restraints END WGHT 0.0336 0.8772 REM Highest difference peak 0.834, deepest hole -0.375, 1-sigma level 0.067 Q1 1 0.5919 0.4220 0.2111 11.00000 0.05 0.83 Q2 1 0.6352 0.5759 0.5157 11.00000 0.05 0.47 Q3 1 0.6408 0.6501 0.4765 11.00000 0.05 0.47 Q4 1 0.6380 0.7322 0.5163 11.00000 0.05 0.47 Q5 1 0.6178 0.5812 0.2588 11.00000 0.05 0.44 Q6 1 0.6259 0.3805 0.3223 11.00000 0.05 0.44 Q7 1 0.6342 0.6553 0.5587 11.00000 0.05 0.43 Q8 1 0.6305 0.3309 0.2710 11.00000 0.05 0.41 Q9 1 0.7057 0.6382 0.5181 11.00000 0.05 0.37 Q10 1 0.4099 0.5803 0.3250 11.00000 0.05 0.36 Q11 1 0.5703 0.6576 0.5221 11.00000 0.05 0.32 Q12 1 0.3674 0.7447 0.3304 11.00000 0.05 0.31 Q13 1 0.6250 1.1464 0.5116 11.00000 0.05 0.30 Q14 1 0.6400 0.3256 0.7597 11.00000 0.05 0.28 Q15 1 0.3692 0.8525 0.3324 11.00000 0.05 0.27 ; _shelx_res_checksum 48571 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, 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 0.63603(2) 0.65255(2) 0.51680(2) 0.01289(6) Uani 1 1 d . . . . . Cl1 Cl 0.78974(5) 0.72546(6) 0.55716(3) 0.02026(13) Uani 1 1 d . . . . . Cl2 Cl 0.72196(5) 0.50202(5) 0.45008(3) 0.01895(13) Uani 1 1 d . . . . . P P 0.63523(5) 0.78687(6) 0.43614(3) 0.01447(13) Uani 1 1 d . . . . . F1 F 0.37388(19) 1.0808(2) 0.68290(13) 0.0480(6) Uani 1 1 d . . . . . F2 F 0.36959(14) 0.94345(19) 0.75281(9) 0.0341(5) Uani 1 1 d . . . . . F3 F 0.25855(16) 0.9481(2) 0.67791(11) 0.0469(6) Uani 1 1 d . . . . . N1 N 0.49712(16) 0.57952(18) 0.49299(11) 0.0138(4) Uani 1 1 d . . . . . N2 N 0.62446(17) 0.5260(2) 0.59129(13) 0.0192(5) Uani 1 1 d . . . . . C1 C 0.7319(2) 0.7672(2) 0.37432(14) 0.0192(5) Uani 1 1 d . . . . . C2 C 0.7105(2) 0.7771(3) 0.30829(15) 0.0240(6) Uani 1 1 d . . . . . H2 H 0.6436 0.7914 0.2946 0.029 Uiso 1 1 calc R U . . . C3 C 0.7863(3) 0.7661(3) 0.26250(16) 0.0311(7) Uani 1 1 d . . . . . H3 H 0.7709 0.7720 0.2177 0.037 Uiso 1 1 calc R U . . . C4 C 0.8843(3) 0.7465(3) 0.28203(17) 0.0330(7) Uani 1 1 d . . . . . H4 H 0.9363 0.7407 0.2507 0.040 Uiso 1 1 calc R U . . . C5 C 0.9068(2) 0.7354(3) 0.34736(17) 0.0310(7) Uani 1 1 d . . . . . H5 H 0.9740 0.7212 0.3607 0.037 Uiso 1 1 calc R U . . . C6 C 0.8310(2) 0.7452(3) 0.39314(15) 0.0247(6) Uani 1 1 d . . . . . H6 H 0.8466 0.7368 0.4378 0.030 Uiso 1 1 calc R U . . . C7 C 0.6488(2) 0.9399(2) 0.46089(13) 0.0173(5) Uani 1 1 d . . . . . C8 C 0.5666(2) 1.0018(2) 0.48544(13) 0.0214(6) Uani 1 1 d . . . . . H8 H 0.5036 0.9635 0.4898 0.026 Uiso 1 1 calc R U . . . C9 C 0.5761(2) 1.1182(3) 0.50342(14) 0.0258(6) Uani 1 1 d . . . . . H9 H 0.5195 1.1597 0.5195 0.031 Uiso 1 1 calc R U . . . C10 C 0.6683(3) 1.1747(3) 0.49807(15) 0.0283(7) Uani 1 1 d . . . . . H10 H 0.6748 1.2551 0.5098 0.034 Uiso 1 1 calc R U . . . C11 C 0.7506(2) 1.1127(3) 0.47539(15) 0.0263(6) Uani 1 1 d . . . . . H11 H 0.8139 1.1506 0.4725 0.032 Uiso 1 1 calc R U . . . C12 C 0.7416(2) 0.9960(2) 0.45691(14) 0.0215(5) Uani 1 1 d . . . . . H12 H 0.7987 0.9543 0.4416 0.026 Uiso 1 1 calc R U . . . C13 C 0.5169(2) 0.7894(2) 0.39169(13) 0.0168(5) Uani 1 1 d . . . . . C14 C 0.4894(2) 0.8916(2) 0.35725(13) 0.0197(5) Uani 1 1 d . . . . . H14 H 0.5330 0.9577 0.3575 0.024 Uiso 1 1 calc R U . . . C15 C 0.4001(2) 0.8972(2) 0.32309(14) 0.0222(6) Uani 1 1 d . . . . . H15 H 0.3830 0.9663 0.2998 0.027 Uiso 1 1 calc R U . . . C16 C 0.3355(2) 0.8010(3) 0.32306(14) 0.0221(5) Uani 1 1 d . . . . . H16 H 0.2736 0.8045 0.3003 0.027 Uiso 1 1 calc R U . . . C17 C 0.36224(19) 0.6996(3) 0.35671(13) 0.0190(6) Uani 1 1 d . . . . . H17 H 0.3180 0.6341 0.3564 0.023 Uiso 1 1 calc R U . . . C18 C 0.4520(2) 0.6920(2) 0.39065(12) 0.0158(5) Uani 1 1 d . . . . . C19 C 0.4766(2) 0.5757(2) 0.42179(12) 0.0154(5) Uani 1 1 d . . . . . H19A H 0.4199 0.5213 0.4141 0.019 Uiso 1 1 calc R U . . . H19B H 0.5363 0.5424 0.3999 0.019 Uiso 1 1 calc R U . . . C20 C 0.50347(18) 0.4536(2) 0.51458(15) 0.0172(4) Uani 1 1 d . . . . . H20A H 0.4352 0.4193 0.5162 0.021 Uiso 1 1 calc R U . . . H20B H 0.5436 0.4080 0.4830 0.021 Uiso 1 1 calc R U . . . C21 C 0.5511(2) 0.4458(2) 0.57998(13) 0.0195(5) Uani 1 1 d . . . . . C22 C 0.5271(3) 0.3607(3) 0.62511(17) 0.0304(7) Uani 1 1 d . . . . . H22 H 0.4752 0.3054 0.6167 0.036 Uiso 1 1 calc R U . . . C23 C 0.5801(3) 0.3575(3) 0.68304(19) 0.0453(10) Uani 1 1 d . . . . . H23 H 0.5655 0.2994 0.7147 0.054 Uiso 1 1 calc R U . . . C24 C 0.6538(3) 0.4395(4) 0.69389(19) 0.0456(10) Uani 1 1 d . . . . . H24 H 0.6905 0.4389 0.7333 0.055 Uiso 1 1 calc R U . . . C25 C 0.6744(3) 0.5233(3) 0.64683(15) 0.0305(7) Uani 1 1 d . . . . . H25 H 0.7254 0.5799 0.6546 0.037 Uiso 1 1 calc R U . . . C26 C 0.4131(2) 0.6398(2) 0.52999(12) 0.0164(6) Uani 1 1 d . . . . . H26A H 0.3639 0.6726 0.4989 0.020 Uiso 1 1 calc R U . . . H26B H 0.3779 0.5813 0.5572 0.020 Uiso 1 1 calc R U . . . C27 C 0.4526(2) 0.7368(2) 0.57211(13) 0.0169(5) Uani 1 1 d . . . . . C28 C 0.5552(2) 0.7606(2) 0.57198(12) 0.0157(5) Uani 1 1 d . . . . . C29 C 0.5913(2) 0.8528(2) 0.61088(14) 0.0194(6) Uani 1 1 d . . . . . H29 H 0.6611 0.8700 0.6114 0.023 Uiso 1 1 calc R U . . . C30 C 0.5263(2) 0.9185(2) 0.64834(14) 0.0211(5) Uani 1 1 d . . . . . H30 H 0.5516 0.9806 0.6744 0.025 Uiso 1 1 calc R U . . . C31 C 0.4239(2) 0.8941(3) 0.64806(13) 0.0212(5) Uani 1 1 d . . . . . C32 C 0.3863(2) 0.8021(3) 0.61007(13) 0.0208(5) Uani 1 1 d . . . . . H32 H 0.3166 0.7844 0.6102 0.025 Uiso 1 1 calc R U . . . C33 C 0.3566(2) 0.9657(3) 0.68956(16) 0.0274(7) Uani 1 1 d . . . . . O1A O 0.6711(12) 0.4771(13) 0.3041(8) 0.086(4) Uiso 0.312(9) 1 d . U P A 1 O1B O 0.593(2) 0.476(2) 0.2734(13) 0.086(4) Uiso 0.181(8) 1 d . U P B 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 0.01304(9) 0.01201(9) 0.01363(9) -0.00004(8) -0.00089(8) 0.00053(6) Cl1 0.0151(3) 0.0232(3) 0.0224(3) -0.0031(3) -0.0027(2) -0.0008(2) Cl2 0.0176(3) 0.0167(3) 0.0226(3) -0.0019(2) 0.0007(2) 0.0042(2) P 0.0155(3) 0.0122(3) 0.0157(3) 0.0003(2) 0.0002(2) -0.0006(2) F1 0.0689(16) 0.0247(10) 0.0504(14) -0.0039(10) 0.0268(11) 0.0150(10) F2 0.0406(12) 0.0427(12) 0.0189(9) -0.0069(8) 0.0052(7) 0.0045(8) F3 0.0270(10) 0.0686(16) 0.0450(13) -0.0270(11) -0.0026(9) 0.0178(10) N1 0.0140(10) 0.0117(10) 0.0156(9) 0.0012(7) -0.0002(8) -0.0001(8) N2 0.0192(11) 0.0196(11) 0.0188(12) 0.0020(9) -0.0015(9) -0.0002(8) C1 0.0233(13) 0.0138(12) 0.0206(13) 0.0010(10) 0.0045(10) -0.0011(10) C2 0.0290(15) 0.0225(14) 0.0204(14) 0.0023(11) 0.0013(11) 0.0043(11) C3 0.0407(19) 0.0301(16) 0.0224(15) 0.0061(12) 0.0091(14) 0.0106(13) C4 0.0357(17) 0.0322(17) 0.0311(17) 0.0085(13) 0.0169(14) 0.0077(13) C5 0.0242(15) 0.0313(16) 0.0374(18) 0.0046(13) 0.0081(13) 0.0051(12) C6 0.0241(14) 0.0270(15) 0.0231(14) 0.0044(11) 0.0026(12) 0.0036(11) C7 0.0217(13) 0.0127(12) 0.0175(13) 0.0027(10) -0.0014(10) -0.0013(9) C8 0.0240(14) 0.0183(13) 0.0221(14) -0.0003(10) -0.0008(11) 0.0005(10) C9 0.0308(15) 0.0198(13) 0.0269(18) -0.0041(10) -0.0039(11) 0.0054(11) C10 0.0380(17) 0.0155(12) 0.0315(17) -0.0016(11) -0.0061(13) -0.0034(12) C11 0.0288(15) 0.0208(14) 0.0293(15) 0.0004(11) -0.0024(12) -0.0075(12) C12 0.0244(13) 0.0180(12) 0.0222(14) 0.0013(10) 0.0003(11) -0.0029(10) C13 0.0198(12) 0.0157(12) 0.0151(12) 0.0001(9) -0.0019(10) 0.0017(10) C14 0.0256(14) 0.0155(12) 0.0179(13) 0.0032(10) 0.0002(10) -0.0006(10) C15 0.0263(14) 0.0197(14) 0.0207(13) 0.0038(10) -0.0001(11) 0.0052(11) C16 0.0210(13) 0.0255(15) 0.0197(13) 0.0019(11) -0.0039(11) 0.0040(11) C17 0.0203(14) 0.0218(15) 0.0149(13) -0.0008(10) 0.0005(9) -0.0023(10) C18 0.0200(12) 0.0158(12) 0.0118(11) -0.0004(9) 0.0007(9) 0.0007(10) C19 0.0194(12) 0.0133(11) 0.0136(12) -0.0002(9) -0.0016(9) -0.0006(9) C20 0.0218(11) 0.0119(10) 0.0178(11) 0.0025(11) -0.0022(12) -0.0007(8) C21 0.0207(13) 0.0168(12) 0.0211(13) 0.0026(10) -0.0028(10) -0.0002(10) C22 0.0355(18) 0.0249(15) 0.0307(17) 0.0097(12) -0.0082(14) -0.0081(12) C23 0.058(3) 0.045(2) 0.0332(19) 0.0239(15) -0.0166(18) -0.0187(18) C24 0.059(2) 0.047(2) 0.0299(19) 0.0164(16) -0.0230(17) -0.0158(18) C25 0.0362(17) 0.0296(16) 0.0256(15) 0.0065(12) -0.0094(13) -0.0065(13) C26 0.0158(12) 0.0168(12) 0.0166(16) 0.0000(9) 0.0017(9) 0.0004(9) C27 0.0201(13) 0.0162(12) 0.0146(12) 0.0006(9) -0.0013(9) 0.0009(9) C28 0.0188(12) 0.0150(12) 0.0133(12) 0.0003(9) -0.0018(9) 0.0006(9) C29 0.0191(14) 0.0212(14) 0.0180(13) -0.0033(10) -0.0021(10) 0.0001(10) C30 0.0283(14) 0.0192(13) 0.0159(13) -0.0048(10) -0.0027(11) 0.0006(10) C31 0.0267(14) 0.0218(13) 0.0150(12) -0.0018(10) 0.0006(10) 0.0062(11) C32 0.0190(12) 0.0265(15) 0.0169(13) -0.0021(11) 0.0003(10) 0.0046(11) C33 0.0300(16) 0.0300(17) 0.0223(15) -0.0082(12) 0.0033(11) 0.0061(12) 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' F F 0.0171 0.0103 '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' 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' O O 0.0106 0.0060 '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 84.37(10) C28 Rh N2 87.96(10) N1 Rh N2 80.54(9) C28 Rh P 90.12(7) N1 Rh P 95.24(6) N2 Rh P 175.52(6) C28 Rh Cl1 92.82(8) N1 Rh Cl1 172.66(6) N2 Rh Cl1 92.60(7) P Rh Cl1 91.54(2) C28 Rh Cl2 173.75(8) N1 Rh Cl2 90.16(6) N2 Rh Cl2 88.16(7) P Rh Cl2 93.40(2) Cl1 Rh Cl2 92.24(2) C7 P C13 102.24(12) C7 P C1 104.05(12) C13 P C1 104.97(12) C7 P Rh 115.98(9) C13 P Rh 112.70(9) C1 P Rh 115.43(9) C19 N1 C20 105.9(2) C19 N1 C26 111.93(19) C20 N1 C26 108.83(19) C19 N1 Rh 113.88(16) C20 N1 Rh 105.06(14) C26 N1 Rh 110.75(15) C25 N2 C21 119.6(3) C25 N2 Rh 127.5(2) C21 N2 Rh 112.67(19) C2 C1 C6 118.5(3) C2 C1 P 122.0(2) C6 C1 P 119.5(2) C3 C2 C1 120.7(3) C3 C2 H2 119.7 C1 C2 H2 119.7 C4 C3 C2 120.1(3) C4 C3 H3 120.0 C2 C3 H3 120.0 C3 C4 C5 120.1(3) C3 C4 H4 119.9 C5 C4 H4 119.9 C6 C5 C4 119.9(3) C6 C5 H5 120.1 C4 C5 H5 120.1 C5 C6 C1 120.7(3) C5 C6 H6 119.6 C1 C6 H6 119.6 C12 C7 C8 119.0(3) C12 C7 P 120.6(2) C8 C7 P 120.4(2) C9 C8 C7 120.6(3) C9 C8 H8 119.7 C7 C8 H8 119.7 C8 C9 C10 120.2(3) C8 C9 H9 119.9 C10 C9 H9 119.9 C11 C10 C9 119.3(3) C11 C10 H10 120.3 C9 C10 H10 120.3 C10 C11 C12 120.9(3) C10 C11 H11 119.6 C12 C11 H11 119.6 C11 C12 C7 119.9(3) C11 C12 H12 120.1 C7 C12 H12 120.1 C18 C13 C14 118.9(2) C18 C13 P 121.73(19) C14 C13 P 119.4(2) C15 C14 C13 121.2(3) C15 C14 H14 119.4 C13 C14 H14 119.4 C14 C15 C16 119.7(3) C14 C15 H15 120.2 C16 C15 H15 120.2 C15 C16 C17 119.5(3) C15 C16 H16 120.2 C17 C16 H16 120.2 C18 C17 C16 121.6(3) C18 C17 H17 119.2 C16 C17 H17 119.2 C17 C18 C13 119.2(2) C17 C18 C19 117.2(2) C13 C18 C19 123.5(2) N1 C19 C18 115.7(2) N1 C19 H19A 108.4 C18 C19 H19A 108.4 N1 C19 H19B 108.4 C18 C19 H19B 108.4 H19A C19 H19B 107.4 C21 C20 N1 110.4(2) 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(3) N2 C21 C20 114.9(2) C22 C21 C20 123.6(3) C21 C22 C23 118.8(3) C21 C22 H22 120.6 C23 C22 H22 120.6 C24 C23 C22 119.1(3) C24 C23 H23 120.4 C22 C23 H23 120.4 C23 C24 C25 119.5(3) C23 C24 H24 120.2 C25 C24 H24 120.2 N2 C25 C24 121.5(3) N2 C25 H25 119.3 C24 C25 H25 119.3 C27 C26 N1 111.5(2) C27 C26 H26A 109.3 N1 C26 H26A 109.3 C27 C26 H26B 109.3 N1 C26 H26B 109.3 H26A C26 H26B 108.0 C28 C27 C32 121.2(2) C28 C27 C26 119.0(2) C32 C27 C26 119.8(2) C27 C28 C29 118.6(2) C27 C28 Rh 114.26(19) C29 C28 Rh 127.1(2) C30 C29 C28 120.7(3) C30 C29 H29 119.7 C28 C29 H29 119.7 C29 C30 C31 120.2(3) C29 C30 H30 119.9 C31 C30 H30 119.9 C30 C31 C32 120.1(3) C30 C31 C33 118.7(3) C32 C31 C33 121.2(3) C27 C32 C31 119.1(3) C27 C32 H32 120.4 C31 C32 H32 120.4 F1 C33 F3 107.2(3) F1 C33 F2 105.2(3) F3 C33 F2 105.8(3) F1 C33 C31 112.0(3) F3 C33 C31 113.7(3) F2 C33 C31 112.4(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Rh C28 1.993(3) Rh N1 2.087(2) Rh N2 2.114(3) Rh P 2.2620(7) Rh Cl1 2.3615(7) Rh Cl2 2.4794(7) P C7 1.824(3) P C13 1.825(3) P C1 1.828(3) F1 C33 1.338(4) F2 C33 1.343(4) F3 C33 1.342(4) N1 C19 1.497(3) N1 C20 1.503(3) N1 C26 1.519(3) N2 C25 1.327(4) N2 C21 1.358(4) C1 C2 1.398(4) C1 C6 1.399(4) C2 C3 1.389(4) C2 H2 0.9500 C3 C4 1.384(5) C3 H3 0.9500 C4 C5 1.389(5) C4 H4 0.9500 C5 C6 1.388(4) C5 H5 0.9500 C6 H6 0.9500 C7 C12 1.394(4) C7 C8 1.398(4) C8 C9 1.382(4) C8 H8 0.9500 C9 C10 1.390(5) C9 H9 0.9500 C10 C11 1.385(5) C10 H10 0.9500 C11 C12 1.388(4) C11 H11 0.9500 C12 H12 0.9500 C13 C18 1.406(4) C13 C14 1.412(4) C14 C15 1.385(4) C14 H14 0.9500 C15 C16 1.393(4) C15 H15 0.9500 C16 C17 1.394(4) C16 H16 0.9500 C17 C18 1.389(4) C17 H17 0.9500 C18 C19 1.508(3) C19 H19A 0.9900 C19 H19B 0.9900 C20 C21 1.496(4) C20 H20A 0.9900 C20 H20B 0.9900 C21 C22 1.382(4) C22 C23 1.391(5) C22 H22 0.9500 C23 C24 1.373(5) C23 H23 0.9500 C24 C25 1.389(5) C24 H24 0.9500 C25 H25 0.9500 C26 C27 1.500(4) C26 H26A 0.9900 C26 H26B 0.9900 C27 C28 1.394(4) C27 C32 1.395(4) C28 C29 1.406(4) C29 C30 1.381(4) C29 H29 0.9500 C30 C31 1.392(4) C30 H30 0.9500 C31 C32 1.401(4) C31 C33 1.485(4) C32 H32 0.9500 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C7 P C1 C2 -96.2(2) C13 P C1 C2 10.8(3) Rh P C1 C2 135.5(2) C7 P C1 C6 81.8(2) C13 P C1 C6 -171.1(2) Rh P C1 C6 -46.4(2) C6 C1 C2 C3 -0.5(4) P C1 C2 C3 177.5(2) C1 C2 C3 C4 -0.7(5) C2 C3 C4 C5 1.3(5) C3 C4 C5 C6 -0.7(5) C4 C5 C6 C1 -0.6(5) C2 C1 C6 C5 1.1(4) P C1 C6 C5 -176.9(2) C13 P C7 C12 -137.6(2) C1 P C7 C12 -28.5(3) Rh P C7 C12 99.4(2) C13 P C7 C8 43.7(3) C1 P C7 C8 152.8(2) Rh P C7 C8 -79.3(2) C12 C7 C8 C9 2.2(4) P C7 C8 C9 -179.1(2) C7 C8 C9 C10 -0.9(4) C8 C9 C10 C11 -0.9(5) C9 C10 C11 C12 1.2(5) C10 C11 C12 C7 0.2(5) C8 C7 C12 C11 -1.9(4) P C7 C12 C11 179.4(2) C7 P C13 C18 -148.3(2) C1 P C13 C18 103.4(2) Rh P C13 C18 -23.1(2) C7 P C13 C14 31.8(2) C1 P C13 C14 -76.5(2) Rh P C13 C14 157.06(19) C18 C13 C14 C15 0.3(4) P C13 C14 C15 -179.8(2) C13 C14 C15 C16 0.6(4) C14 C15 C16 C17 -0.9(4) C15 C16 C17 C18 0.2(4) C16 C17 C18 C13 0.8(4) C16 C17 C18 C19 -176.2(3) C14 C13 C18 C17 -1.0(4) P C13 C18 C17 179.1(2) C14 C13 C18 C19 175.7(2) P C13 C18 C19 -4.1(4) C20 N1 C19 C18 171.4(2) C26 N1 C19 C18 52.9(3) Rh N1 C19 C18 -73.6(2) C17 C18 C19 N1 -124.4(3) C13 C18 C19 N1 58.8(3) C19 N1 C20 C21 164.4(2) C26 N1 C20 C21 -75.1(2) Rh N1 C20 C21 43.6(2) C25 N2 C21 C22 -0.1(5) Rh N2 C21 C22 -175.4(3) C25 N2 C21 C20 -177.1(3) Rh N2 C21 C20 7.5(3) N1 C20 C21 N2 -35.0(3) N1 C20 C21 C22 148.0(3) N2 C21 C22 C23 -0.4(5) C20 C21 C22 C23 176.4(3) C21 C22 C23 C24 0.7(6) C22 C23 C24 C25 -0.4(7) C21 N2 C25 C24 0.4(5) Rh N2 C25 C24 175.0(3) C23 C24 C25 N2 -0.1(7) C19 N1 C26 C27 -126.9(2) C20 N1 C26 C27 116.4(2) Rh N1 C26 C27 1.3(2) N1 C26 C27 C28 0.9(3) N1 C26 C27 C32 -179.7(2) C32 C27 C28 C29 -0.3(4) C26 C27 C28 C29 179.1(2) C32 C27 C28 Rh 177.8(2) C26 C27 C28 Rh -2.8(3) C27 C28 C29 C30 -0.1(4) Rh C28 C29 C30 -178.0(2) C28 C29 C30 C31 0.1(4) C29 C30 C31 C32 0.4(4) C29 C30 C31 C33 179.3(3) C28 C27 C32 C31 0.8(4) C26 C27 C32 C31 -178.6(2) C30 C31 C32 C27 -0.8(4) C33 C31 C32 C27 -179.7(3) C30 C31 C33 F1 48.0(4) C32 C31 C33 F1 -133.1(3) C30 C31 C33 F3 169.7(3) C32 C31 C33 F3 -11.4(4) C30 C31 C33 F2 -70.1(4) C32 C31 C33 F2 108.7(3)