data_General _audit_creation_date 'Wed Oct 9 15:53:35 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_PNP-Rh-Cl _publ_requested_journal Organometallics _publ_contact_author_name 'Fumiyuki Ozawa' _publ_contact_author_address 'Institute for Chemical Research, Kyoto University, Uji, Kyoto 611-0011, Japan' _publ_contact_author_email ozawa@scl.kyoto-u.ac.jp _publ_contact_author_phone +81-774-38-3035 _publ_contact_author_fax ;+81-774-38-3039 ; loop_ _publ_author_name _publ_author_address 'Ozawa, Fumiyuki ' 'Institute for Chemical Research, Kyoto University, Uji, Kyoto 611-0011, Japan' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C51 H83 Cl N O2 P2 Rh' _chemical_formula_moiety 'C51 H83 Cl N O2 P2 Rh' _chemical_formula_weight 942.53 _chemical_melting_point '468' #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _cell_length_a 16.980(1) _cell_length_b 33.843(2) _cell_length_c 18.534(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10651(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 20586 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description Prism _exptl_crystal_colour Dark_Green _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 0.870 _diffrn_radiation_probe x-ray #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'rotating-anode X-ray tube' _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 83158 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12156 _reflns_number_gt 8039 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1831 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8039 _refine_ls_number_parameters 523 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0050 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.96 _refine_diff_density_min -0.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh(1) Rh 0.93549(2) 0.12588(1) 0.17585(2) 0.0406(1) Uani 1.00 d . . . Cl(1) Cl 0.95269(9) 0.13094(3) 0.05253(6) 0.0644(3) Uani 1.00 d . . . P(1) P 0.99582(7) 0.06816(3) 0.19469(6) 0.0415(2) Uani 1.00 d . . . P(2) P 0.86478(7) 0.18055(3) 0.19395(6) 0.0444(3) Uani 1.00 d . . . O(1) O 1.0457(8) -0.0314(6) 0.4106(6) 0.274(8) Uani 1.00 d . . . O(2) O 0.8107(3) 0.2710(2) 0.3774(2) 0.111(2) Uani 1.00 d . . . N(1) N 0.9273(2) 0.12396(8) 0.2863(2) 0.0379(7) Uani 1.00 d . . . C(1) C 1.0463(2) 0.0251(1) 0.1574(2) 0.0391(8) Uani 1.00 d . . . C(2) C 1.0019(3) -0.0091(1) 0.1374(2) 0.0430(9) Uani 1.00 d . . . C(3) C 1.0415(3) -0.0453(1) 0.1355(2) 0.049(1) Uani 1.00 d . . . C(4) C 1.1206(3) -0.0491(1) 0.1503(2) 0.0479(10) Uani 1.00 d . . . C(5) C 1.1631(3) -0.0146(1) 0.1610(2) 0.049(1) Uani 1.00 d . . . C(6) C 1.1290(3) 0.0229(1) 0.1629(2) 0.0418(9) Uani 1.00 d . . . C(7) C 0.9143(3) -0.0092(1) 0.1171(3) 0.054(1) Uani 1.00 d . . . C(8) C 0.8647(4) -0.0168(4) 0.1825(5) 0.159(4) Uani 1.00 d . . . C(9) C 0.8872(5) 0.0275(2) 0.0793(5) 0.136(4) Uani 1.00 d . . . C(10) C 0.8962(4) -0.0424(2) 0.0641(5) 0.135(4) Uani 1.00 d . . . C(11) C 1.1621(3) -0.0892(1) 0.1525(3) 0.059(1) Uani 1.00 d . . . C(12) C 1.1044(4) -0.1233(1) 0.1518(4) 0.086(2) Uani 1.00 d . . . C(13) C 1.2136(4) -0.0931(2) 0.0855(4) 0.090(2) Uani 1.00 d . . . C(14) C 1.2134(5) -0.0921(2) 0.2192(4) 0.113(3) Uani 1.00 d . . . C(15) C 1.1860(3) 0.0586(1) 0.1700(2) 0.050(1) Uani 1.00 d . . . C(16) C 1.2626(4) 0.0495(2) 0.1305(4) 0.094(2) Uani 1.00 d . . . C(17) C 1.2074(4) 0.0652(2) 0.2491(3) 0.079(2) Uani 1.00 d . . . C(18) C 1.1541(3) 0.0961(1) 0.1369(3) 0.069(1) Uani 1.00 d . . . C(19) C 0.9974(3) 0.0626(1) 0.2838(2) 0.0471(10) Uani 1.00 d . . . C(20) C 0.9611(3) 0.0935(1) 0.3253(2) 0.0411(8) Uani 1.00 d . . . C(21) C 0.9590(3) 0.0929(1) 0.4007(2) 0.050(1) Uani 1.00 d . . . C(22) C 0.9240(3) 0.1237(1) 0.4385(2) 0.053(1) Uani 1.00 d . . . C(23) C 0.8895(3) 0.1536(1) 0.3991(2) 0.052(1) Uani 1.00 d . . . C(24) C 0.8914(2) 0.1538(1) 0.3246(2) 0.0415(9) Uani 1.00 d . . . C(25) C 0.8557(3) 0.1849(1) 0.2830(2) 0.0478(10) Uani 1.00 d . . . C(26) C 0.8171(3) 0.2222(1) 0.1489(2) 0.0426(9) Uani 1.00 d . . . C(27) C 0.8580(3) 0.2583(1) 0.1400(2) 0.0432(9) Uani 1.00 d . . . C(28) C 0.8156(3) 0.2912(1) 0.1161(2) 0.0471(10) Uani 1.00 d . . . C(29) C 0.7364(3) 0.2898(1) 0.0987(2) 0.0469(10) Uani 1.00 d . . . C(30) C 0.6992(3) 0.2536(1) 0.1037(2) 0.0484(10) Uani 1.00 d . . . C(31) C 0.7365(3) 0.2194(1) 0.1280(2) 0.0463(9) Uani 1.00 d . . . C(32) C 0.9462(3) 0.2660(1) 0.1569(2) 0.050(1) Uani 1.00 d . . . C(33) C 0.9784(4) 0.3001(2) 0.1115(4) 0.095(2) Uani 1.00 d . . . C(34) C 0.9548(4) 0.2767(2) 0.2367(4) 0.098(2) Uani 1.00 d . . . C(35) C 1.0001(3) 0.2309(2) 0.1401(4) 0.074(1) Uani 1.00 d . . . C(36) C 0.6903(3) 0.3258(1) 0.0728(3) 0.058(1) Uani 1.00 d . . . C(37) C 0.7394(3) 0.3628(1) 0.0669(3) 0.074(2) Uani 1.00 d . . . C(38) C 0.6218(4) 0.3340(2) 0.1246(4) 0.095(2) Uani 1.00 d . . . C(39) C 0.6571(4) 0.3171(2) -0.0027(4) 0.087(2) Uani 1.00 d . . . C(40) C 0.6856(3) 0.1809(1) 0.1292(3) 0.061(1) Uani 1.00 d . . . C(41) C 0.6582(4) 0.1727(2) 0.2061(4) 0.093(2) Uani 1.00 d . . . C(42) C 0.7293(4) 0.1453(2) 0.0986(3) 0.079(2) Uani 1.00 d . . . C(43) C 0.6117(4) 0.1855(2) 0.0827(5) 0.125(3) Uani 1.00 d . . . C(44) C 1.030(2) -0.0613(6) 0.368(2) 0.28(1) Uani 1.00 d . . . C(45) C 0.953(1) -0.0764(8) 0.366(1) 0.31(1) Uani 1.00 d . . . C(46) C 1.126(1) -0.0249(5) 0.415(1) 0.26(1) Uani 1.00 d . . . C(47) C 1.135(1) 0.0080(7) 0.455(1) 0.31(1) Uani 1.00 d . . . C(48) C 0.8469(5) 0.2761(2) 0.4446(3) 0.099(2) Uani 1.00 d . . . C(49) C 0.9307(5) 0.2705(3) 0.4370(4) 0.118(3) Uani 1.00 d . . . C(50) C 0.7293(5) 0.2812(3) 0.3745(5) 0.115(3) Uani 1.00 d . . . C(51) C 0.7050(5) 0.2844(3) 0.3011(5) 0.120(3) Uani 1.00 d . . . H(1) H 0.8282 0.2078 0.3113 0.0593 Uiso 1.00 calc . . . H(2) H 0.8618 0.1776 0.4297 0.0593 Uiso 1.00 calc . . . H(3) H 0.9268 0.1233 0.4847 0.0593 Uiso 1.00 calc . . . H(4) H 0.9831 0.0705 0.4291 0.0593 Uiso 1.00 calc . . . H(5) H 1.0176 0.0390 0.3055 0.0593 Uiso 1.00 calc . . . H(6) H 0.6420 0.2514 0.0870 0.0593 Uiso 1.00 calc . . . H(7) H 0.8434 0.3181 0.1169 0.0593 Uiso 1.00 calc . . . H(8) H 1.0146 -0.0705 0.1236 0.0593 Uiso 1.00 calc . . . H(9) H 1.2213 -0.0168 0.1724 0.0593 Uiso 1.00 calc . . . H(10) H 0.8766 0.0033 0.2195 0.2021 Uiso 1.00 calc . . . H(11) H 0.8119 -0.0174 0.1740 0.2021 Uiso 1.00 calc . . . H(12) H 0.8814 -0.0418 0.2052 0.2021 Uiso 1.00 calc . . . H(13) H 0.8963 0.0498 0.1115 0.1693 Uiso 1.00 calc . . . H(14) H 0.9161 0.0317 0.0368 0.1693 Uiso 1.00 calc . . . H(15) H 0.8328 0.0261 0.0697 0.1693 Uiso 1.00 calc . . . H(16) H 0.8434 -0.0432 0.0509 0.1539 Uiso 1.00 calc . . . H(17) H 0.9268 -0.0373 0.0185 0.1539 Uiso 1.00 calc . . . H(18) H 0.9140 -0.0670 0.0813 0.1539 Uiso 1.00 calc . . . H(19) H 1.0717 -0.1217 0.1944 0.1013 Uiso 1.00 calc . . . H(20) H 1.0718 -0.1216 0.1107 0.1013 Uiso 1.00 calc . . . H(21) H 1.1317 -0.1476 0.1525 0.1013 Uiso 1.00 calc . . . H(22) H 1.2403 -0.1175 0.0843 0.1126 Uiso 1.00 calc . . . H(23) H 1.1803 -0.0916 0.0424 0.1126 Uiso 1.00 calc . . . H(24) H 1.2503 -0.0720 0.0827 0.1126 Uiso 1.00 calc . . . H(25) H 1.1825 -0.0909 0.2624 0.1443 Uiso 1.00 calc . . . H(26) H 1.2424 -0.1165 0.2198 0.1443 Uiso 1.00 calc . . . H(27) H 1.2509 -0.0709 0.2206 0.1443 Uiso 1.00 calc . . . H(28) H 1.2882 0.0260 0.1493 0.1111 Uiso 1.00 calc . . . H(29) H 1.2537 0.0447 0.0798 0.1111 Uiso 1.00 calc . . . H(30) H 1.3002 0.0706 0.1341 0.1111 Uiso 1.00 calc . . . H(31) H 1.2308 0.0424 0.2700 0.0954 Uiso 1.00 calc . . . H(32) H 1.2421 0.0871 0.2547 0.0954 Uiso 1.00 calc . . . H(33) H 1.1599 0.0711 0.2765 0.0954 Uiso 1.00 calc . . . H(34) H 1.1894 0.1173 0.1408 0.0827 Uiso 1.00 calc . . . H(35) H 1.1429 0.0917 0.0860 0.0827 Uiso 1.00 calc . . . H(36) H 1.1049 0.1032 0.1592 0.0827 Uiso 1.00 calc . . . H(37) H 1.0300 0.3058 0.1209 0.1150 Uiso 1.00 calc . . . H(38) H 0.9741 0.2925 0.0593 0.1150 Uiso 1.00 calc . . . H(39) H 0.9454 0.3229 0.1161 0.1150 Uiso 1.00 calc . . . H(40) H 0.9411 0.2548 0.2671 0.1208 Uiso 1.00 calc . . . H(41) H 1.0092 0.2834 0.2474 0.1208 Uiso 1.00 calc . . . H(42) H 0.9231 0.2986 0.2493 0.1208 Uiso 1.00 calc . . . H(43) H 0.9842 0.2083 0.1689 0.0878 Uiso 1.00 calc . . . H(44) H 0.9978 0.2239 0.0912 0.0878 Uiso 1.00 calc . . . H(45) H 1.0531 0.2371 0.1532 0.0878 Uiso 1.00 calc . . . H(46) H 0.7612 0.3695 0.1140 0.0903 Uiso 1.00 calc . . . H(47) H 0.7841 0.3586 0.0355 0.0903 Uiso 1.00 calc . . . H(48) H 0.7104 0.3845 0.0500 0.0903 Uiso 1.00 calc . . . H(49) H 0.6428 0.3407 0.1717 0.1144 Uiso 1.00 calc . . . H(50) H 0.5919 0.3561 0.1082 0.1144 Uiso 1.00 calc . . . H(51) H 0.5891 0.3118 0.1292 0.1144 Uiso 1.00 calc . . . H(52) H 0.6255 0.3382 -0.0196 0.0998 Uiso 1.00 calc . . . H(53) H 0.6990 0.3126 -0.0366 0.0998 Uiso 1.00 calc . . . H(54) H 0.6253 0.2935 -0.0015 0.0998 Uiso 1.00 calc . . . H(55) H 0.6269 0.1944 0.2242 0.1097 Uiso 1.00 calc . . . H(56) H 0.6277 0.1494 0.2086 0.1097 Uiso 1.00 calc . . . H(57) H 0.7024 0.1699 0.2388 0.1097 Uiso 1.00 calc . . . H(58) H 0.6970 0.1225 0.0998 0.0952 Uiso 1.00 calc . . . H(59) H 0.7451 0.1503 0.0500 0.0952 Uiso 1.00 calc . . . H(60) H 0.7764 0.1399 0.1263 0.0952 Uiso 1.00 calc . . . H(61) H 0.5808 0.2075 0.0942 0.1466 Uiso 1.00 calc . . . H(62) H 0.6289 0.1902 0.0304 0.1466 Uiso 1.00 calc . . . H(63) H 0.5810 0.1623 0.0803 0.1466 Uiso 1.00 calc . . . H(64) H 0.9065 -0.0583 0.3694 0.3768 Uiso 1.00 calc . . . H(65) H 0.9322 -0.0956 0.3268 0.3768 Uiso 1.00 calc . . . H(66) H 0.9455 -0.0935 0.4095 0.3768 Uiso 1.00 calc . . . H(67) H 1.1960 0.0142 0.4564 0.4476 Uiso 1.00 calc . . . H(68) H 1.1162 0.0303 0.4281 0.4476 Uiso 1.00 calc . . . H(69) H 1.1194 0.0068 0.5000 0.4476 Uiso 1.00 calc . . . H(70) H 0.9424 0.2458 0.4197 0.1345 Uiso 1.00 calc . . . H(71) H 0.9507 0.2909 0.4067 0.1345 Uiso 1.00 calc . . . H(72) H 0.9559 0.2741 0.4844 0.1345 Uiso 1.00 calc . . . H(73) H 0.7367 0.3045 0.2792 0.1350 Uiso 1.00 calc . . . H(74) H 0.7146 0.2600 0.2788 0.1350 Uiso 1.00 calc . . . H(75) H 0.6521 0.2914 0.2998 0.1350 Uiso 1.00 calc . . . H(76) H 1.0170 -0.0478 0.3101 0.3396 Uiso 1.00 calc . . . H(77) H 1.0560 -0.0829 0.3504 0.3396 Uiso 1.00 calc . . . H(78) H 1.1546 -0.0466 0.4404 0.2862 Uiso 1.00 calc . . . H(79) H 1.1513 -0.0231 0.3686 0.2862 Uiso 1.00 calc . . . H(80) H 0.8359 0.3012 0.4660 0.1185 Uiso 1.00 calc . . . H(81) H 0.8277 0.2561 0.4785 0.1185 Uiso 1.00 calc . . . H(82) H 0.6986 0.2616 0.3962 0.1363 Uiso 1.00 calc . . . H(83) H 0.7201 0.3062 0.3968 0.1363 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0465(2) 0.0347(2) 0.0406(2) 0.0076(1) 0.0010(1) 0.0020(1) Cl(1) 0.0888(10) 0.0623(7) 0.0422(5) 0.0054(6) 0.0032(6) 0.0049(5) P(1) 0.0432(6) 0.0342(5) 0.0470(5) 0.0073(4) 0.0009(5) 0.0003(4) P(2) 0.0467(7) 0.0363(5) 0.0501(6) 0.0114(4) 0.0005(5) 0.0048(4) O(1) 0.145(9) 0.50(3) 0.177(9) 0.07(1) 0.000(8) -0.03(1) O(2) 0.087(4) 0.163(4) 0.083(3) 0.021(3) -0.003(3) -0.041(3) N(1) 0.036(2) 0.037(1) 0.041(2) 0.002(1) 0.002(1) 0.002(1) C(1) 0.038(2) 0.029(2) 0.050(2) 0.005(1) 0.005(2) -0.001(1) C(2) 0.041(2) 0.036(2) 0.051(2) -0.003(2) 0.003(2) 0.000(2) C(3) 0.052(3) 0.034(2) 0.061(3) -0.002(2) -0.004(2) -0.006(2) C(4) 0.057(3) 0.035(2) 0.052(2) 0.010(2) -0.004(2) -0.007(2) C(5) 0.042(2) 0.038(2) 0.066(3) 0.008(2) -0.008(2) -0.004(2) C(6) 0.040(2) 0.035(2) 0.051(2) 0.000(2) -0.002(2) -0.005(2) C(7) 0.037(2) 0.045(2) 0.080(3) -0.005(2) -0.001(2) -0.001(2) C(8) 0.041(4) 0.32(1) 0.117(6) -0.020(6) 0.010(4) 0.052(7) C(9) 0.100(6) 0.077(4) 0.231(10) -0.030(4) -0.109(6) 0.052(5) C(10) 0.072(5) 0.118(6) 0.215(9) 0.015(4) -0.059(5) -0.084(6) C(11) 0.068(3) 0.034(2) 0.074(3) 0.013(2) -0.013(3) -0.006(2) C(12) 0.105(5) 0.034(2) 0.120(5) 0.012(3) -0.002(4) 0.004(3) C(13) 0.093(5) 0.066(3) 0.111(5) 0.026(3) 0.013(4) -0.015(3) C(14) 0.154(7) 0.064(3) 0.122(5) 0.046(4) -0.064(5) -0.012(3) C(15) 0.040(2) 0.043(2) 0.067(3) -0.006(2) -0.001(2) -0.005(2) C(16) 0.055(4) 0.067(3) 0.160(6) -0.015(3) 0.028(4) -0.017(4) C(17) 0.077(4) 0.068(3) 0.091(4) -0.016(3) -0.030(3) -0.009(3) C(18) 0.051(3) 0.049(2) 0.106(4) -0.017(2) -0.010(3) 0.011(3) C(19) 0.045(3) 0.041(2) 0.055(2) 0.009(2) -0.004(2) 0.005(2) C(20) 0.039(2) 0.042(2) 0.042(2) 0.001(2) 0.000(2) 0.005(2) C(21) 0.046(3) 0.057(2) 0.045(2) 0.004(2) -0.005(2) 0.007(2) C(22) 0.054(3) 0.061(3) 0.043(2) 0.008(2) 0.007(2) 0.002(2) C(23) 0.055(3) 0.052(2) 0.049(2) 0.006(2) 0.006(2) -0.005(2) C(24) 0.035(2) 0.043(2) 0.047(2) 0.003(2) 0.003(2) 0.000(2) C(25) 0.052(3) 0.038(2) 0.053(2) 0.012(2) 0.006(2) -0.001(2) C(26) 0.045(3) 0.034(2) 0.049(2) 0.008(2) 0.000(2) 0.006(2) C(27) 0.043(2) 0.038(2) 0.050(2) 0.004(2) 0.000(2) 0.003(2) C(28) 0.045(3) 0.040(2) 0.056(2) 0.004(2) 0.001(2) 0.004(2) C(29) 0.044(3) 0.045(2) 0.052(2) 0.006(2) 0.002(2) 0.008(2) C(30) 0.038(2) 0.043(2) 0.064(3) 0.005(2) -0.001(2) 0.010(2) C(31) 0.040(2) 0.039(2) 0.059(2) 0.001(2) 0.002(2) 0.011(2) C(32) 0.041(3) 0.049(2) 0.059(2) 0.001(2) -0.005(2) -0.002(2) C(33) 0.055(4) 0.086(4) 0.144(6) -0.009(3) -0.013(4) 0.046(4) C(34) 0.073(4) 0.131(5) 0.091(4) -0.010(4) -0.004(4) -0.050(4) C(35) 0.041(3) 0.071(3) 0.111(4) 0.003(2) 0.004(3) -0.007(3) C(36) 0.052(3) 0.043(2) 0.080(3) 0.014(2) 0.008(2) 0.017(2) C(37) 0.071(4) 0.043(2) 0.108(4) 0.013(2) 0.011(3) 0.020(3) C(38) 0.072(4) 0.071(3) 0.142(6) 0.028(3) 0.037(4) 0.031(4) C(39) 0.091(5) 0.072(3) 0.098(4) 0.009(3) -0.032(4) 0.029(3) C(40) 0.049(3) 0.041(2) 0.094(4) -0.001(2) -0.007(3) 0.012(2) C(41) 0.079(4) 0.070(3) 0.131(5) -0.017(3) 0.035(4) 0.022(4) C(42) 0.075(4) 0.056(3) 0.106(4) -0.011(3) -0.005(3) -0.011(3) C(43) 0.074(5) 0.077(4) 0.224(9) -0.027(3) -0.075(5) 0.043(5) C(44) 0.29(3) 0.22(2) 0.32(3) -0.02(2) 0.15(3) -0.03(2) C(45) 0.18(2) 0.49(4) 0.26(2) 0.02(2) -0.06(2) 0.07(2) C(46) 0.20(2) 0.21(2) 0.37(3) 0.02(1) 0.14(2) 0.07(2) C(47) 0.18(2) 0.39(3) 0.37(3) 0.13(2) -0.07(2) 0.05(2) C(48) 0.134(7) 0.097(4) 0.065(4) -0.010(4) 0.005(4) -0.008(3) C(49) 0.117(7) 0.150(7) 0.086(5) 0.003(5) -0.029(5) -0.002(5) C(50) 0.079(5) 0.155(7) 0.113(6) 0.018(5) 0.027(4) -0.004(5) C(51) 0.090(6) 0.163(7) 0.108(6) 0.016(5) 0.008(5) 0.009(5) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) Cl(1) 2.311(1) . . yes Rh(1) P(1) 2.233(1) . . yes Rh(1) P(2) 2.231(1) . . yes Rh(1) N(1) 2.053(3) . . yes P(1) C(1) 1.826(4) . . yes P(1) C(19) 1.662(4) . . yes P(2) C(25) 1.664(4) . . yes P(2) C(26) 1.827(4) . . yes O(1) C(44) 1.31(3) . . yes O(1) C(46) 1.38(3) . . yes O(2) C(48) 1.401(8) . . yes O(2) C(50) 1.425(10) . . yes N(1) C(20) 1.384(5) . . yes N(1) C(24) 1.375(5) . . yes C(1) C(2) 1.429(5) . . yes C(1) C(6) 1.410(6) . . yes C(2) C(3) 1.398(6) . . yes C(2) C(7) 1.534(6) . . yes C(3) C(4) 1.378(7) . . yes C(4) C(5) 1.385(6) . . yes C(4) C(11) 1.528(6) . . yes C(5) C(6) 1.396(5) . . yes C(6) C(15) 1.553(6) . . yes C(7) C(8) 1.499(10) . . yes C(7) C(9) 1.495(9) . . yes C(7) C(10) 1.524(10) . . yes C(11) C(12) 1.515(7) . . yes C(11) C(13) 1.525(9) . . yes C(11) C(14) 1.515(9) . . yes C(15) C(16) 1.523(8) . . yes C(15) C(17) 1.528(7) . . yes C(15) C(18) 1.509(6) . . yes C(19) C(20) 1.437(6) . . yes C(20) C(21) 1.398(6) . . yes C(21) C(22) 1.390(6) . . yes C(22) C(23) 1.379(6) . . yes C(23) C(24) 1.380(6) . . yes C(24) C(25) 1.441(6) . . yes C(26) C(27) 1.416(5) . . yes C(26) C(31) 1.426(6) . . yes C(27) C(28) 1.398(6) . . yes C(27) C(32) 1.551(6) . . yes C(28) C(29) 1.385(6) . . yes C(29) C(30) 1.382(6) . . yes C(29) C(36) 1.526(6) . . yes C(30) C(31) 1.395(6) . . yes C(31) C(40) 1.563(6) . . yes C(32) C(33) 1.528(8) . . yes C(32) C(34) 1.529(8) . . yes C(32) C(35) 1.532(7) . . yes C(36) C(37) 1.507(7) . . yes C(36) C(38) 1.535(8) . . yes C(36) C(39) 1.538(8) . . yes C(40) C(41) 1.525(9) . . yes C(40) C(42) 1.522(7) . . yes C(40) C(43) 1.530(9) . . yes C(44) C(45) 1.41(4) . . yes C(46) C(47) 1.35(3) . . yes C(48) C(49) 1.44(1) . . yes C(50) C(51) 1.43(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Rh(1) P(1) 99.29(4) . . . yes Cl(1) Rh(1) P(2) 98.93(4) . . . yes Cl(1) Rh(1) N(1) 175.82(9) . . . yes P(1) Rh(1) P(2) 161.58(4) . . . yes P(1) Rh(1) N(1) 81.23(8) . . . yes P(2) Rh(1) N(1) 80.78(8) . . . yes Rh(1) P(1) C(1) 148.7(1) . . . yes Rh(1) P(1) C(19) 105.2(1) . . . yes C(1) P(1) C(19) 106.1(2) . . . yes Rh(1) P(2) C(25) 105.9(1) . . . yes Rh(1) P(2) C(26) 144.0(1) . . . yes C(25) P(2) C(26) 110.1(2) . . . yes C(44) O(1) C(46) 110(1) . . . yes C(48) O(2) C(50) 115.4(6) . . . yes Rh(1) N(1) C(20) 121.1(2) . . . yes Rh(1) N(1) C(24) 121.4(2) . . . yes C(20) N(1) C(24) 117.4(3) . . . yes P(1) C(1) C(2) 119.7(3) . . . yes P(1) C(1) C(6) 118.9(3) . . . yes C(2) C(1) C(6) 120.0(3) . . . yes C(1) C(2) C(3) 117.5(4) . . . yes C(1) C(2) C(7) 125.2(3) . . . yes C(3) C(2) C(7) 117.2(4) . . . yes C(2) C(3) C(4) 123.1(4) . . . yes C(3) C(4) C(5) 117.1(4) . . . yes C(3) C(4) C(11) 122.6(4) . . . yes C(5) C(4) C(11) 120.2(4) . . . yes C(4) C(5) C(6) 123.7(4) . . . yes C(1) C(6) C(5) 117.4(3) . . . yes C(1) C(6) C(15) 125.8(3) . . . yes C(5) C(6) C(15) 116.8(4) . . . yes C(2) C(7) C(8) 110.2(5) . . . yes C(2) C(7) C(9) 114.3(4) . . . yes C(2) C(7) C(10) 110.9(4) . . . yes C(8) C(7) C(9) 110.4(6) . . . yes C(8) C(7) C(10) 106.2(6) . . . yes C(9) C(7) C(10) 104.4(6) . . . yes C(4) C(11) C(12) 112.2(4) . . . yes C(4) C(11) C(13) 108.6(4) . . . yes C(4) C(11) C(14) 110.2(4) . . . yes C(12) C(11) C(13) 107.4(4) . . . yes C(12) C(11) C(14) 109.2(5) . . . yes C(13) C(11) C(14) 109.2(5) . . . yes C(6) C(15) C(16) 109.6(4) . . . yes C(6) C(15) C(17) 110.1(4) . . . yes C(6) C(15) C(18) 113.3(4) . . . yes C(16) C(15) C(17) 106.7(5) . . . yes C(16) C(15) C(18) 106.3(4) . . . yes C(17) C(15) C(18) 110.6(4) . . . yes P(1) C(19) C(20) 116.2(3) . . . yes N(1) C(20) C(19) 116.2(3) . . . yes N(1) C(20) C(21) 121.4(4) . . . yes C(19) C(20) C(21) 122.4(4) . . . yes C(20) C(21) C(22) 120.3(4) . . . yes C(21) C(22) C(23) 117.6(4) . . . yes C(22) C(23) C(24) 121.6(4) . . . yes N(1) C(24) C(23) 121.5(4) . . . yes N(1) C(24) C(25) 116.6(3) . . . yes C(23) C(24) C(25) 121.9(4) . . . yes P(2) C(25) C(24) 115.2(3) . . . yes P(2) C(26) C(27) 120.1(3) . . . yes P(2) C(26) C(31) 119.9(3) . . . yes C(27) C(26) C(31) 119.8(3) . . . yes C(26) C(27) C(28) 118.2(4) . . . yes C(26) C(27) C(32) 126.5(4) . . . yes C(28) C(27) C(32) 115.3(3) . . . yes C(27) C(28) C(29) 123.2(4) . . . yes C(28) C(29) C(30) 117.3(4) . . . yes C(28) C(29) C(36) 123.0(4) . . . yes C(30) C(29) C(36) 119.7(4) . . . yes C(29) C(30) C(31) 123.4(4) . . . yes C(26) C(31) C(30) 117.9(3) . . . yes C(26) C(31) C(40) 125.6(3) . . . yes C(30) C(31) C(40) 116.5(4) . . . yes C(27) C(32) C(33) 111.1(4) . . . yes C(27) C(32) C(34) 109.1(4) . . . yes C(27) C(32) C(35) 113.9(4) . . . yes C(33) C(32) C(34) 108.6(4) . . . yes C(33) C(32) C(35) 105.0(4) . . . yes C(34) C(32) C(35) 108.9(4) . . . yes C(29) C(36) C(37) 113.7(4) . . . yes C(29) C(36) C(38) 109.5(4) . . . yes C(29) C(36) C(39) 108.7(4) . . . yes C(37) C(36) C(38) 108.5(4) . . . yes C(37) C(36) C(39) 107.3(4) . . . yes C(38) C(36) C(39) 109.0(5) . . . yes C(31) C(40) C(41) 109.5(4) . . . yes C(31) C(40) C(42) 112.6(4) . . . yes C(31) C(40) C(43) 111.2(4) . . . yes C(41) C(40) C(42) 110.6(4) . . . yes C(41) C(40) C(43) 107.1(5) . . . yes C(42) C(40) C(43) 105.7(5) . . . yes O(1) C(44) C(45) 119(2) . . . yes O(1) C(46) C(47) 105(1) . . . yes O(2) C(48) C(49) 109.3(6) . . . yes O(2) C(50) C(51) 109.5(7) . . . yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh(1) P(1) C(1) C(2) -90.2(4) . . . . yes Rh(1) P(1) C(1) C(6) 103.0(4) . . . . yes Rh(1) P(1) C(19) C(20) 0.9(4) . . . . yes Rh(1) P(2) C(25) C(24) -1.6(3) . . . . yes Rh(1) P(2) C(26) C(27) -93.1(4) . . . . yes Rh(1) P(2) C(26) C(31) 92.0(4) . . . . yes Rh(1) N(1) C(20) C(19) -3.7(5) . . . . yes Rh(1) N(1) C(20) C(21) 177.0(3) . . . . yes Rh(1) N(1) C(24) C(23) -176.5(3) . . . . yes Rh(1) N(1) C(24) C(25) 3.8(5) . . . . yes Cl(1) Rh(1) P(1) C(1) -3.5(3) . . . . yes Cl(1) Rh(1) P(1) C(19) 173.8(2) . . . . yes Cl(1) Rh(1) P(2) C(25) -173.2(2) . . . . yes Cl(1) Rh(1) P(2) C(26) 3.8(2) . . . . yes Cl(1) Rh(1) N(1) C(20) -94(1) . . . . yes Cl(1) Rh(1) N(1) C(24) 82(1) . . . . yes P(1) Rh(1) P(2) C(25) 15.0(2) . . . . yes P(1) Rh(1) P(2) C(26) -167.9(2) . . . . yes P(1) Rh(1) N(1) C(20) 3.3(3) . . . . yes P(1) Rh(1) N(1) C(24) -179.8(3) . . . . yes P(1) C(1) C(2) C(3) -156.3(3) . . . . yes P(1) C(1) C(2) C(7) 24.4(6) . . . . yes P(1) C(1) C(6) C(5) 155.6(3) . . . . yes P(1) C(1) C(6) C(15) -25.3(5) . . . . yes P(1) C(19) C(20) N(1) 1.5(5) . . . . yes P(1) C(19) C(20) C(21) -179.2(3) . . . . yes P(2) Rh(1) P(1) C(1) 168.2(3) . . . . yes P(2) Rh(1) P(1) C(19) -14.5(2) . . . . yes P(2) Rh(1) N(1) C(20) 179.4(3) . . . . yes P(2) Rh(1) N(1) C(24) -3.8(3) . . . . yes P(2) C(25) C(24) N(1) -1.1(5) . . . . yes P(2) C(25) C(24) C(23) 179.2(3) . . . . yes P(2) C(26) C(27) C(28) -169.7(3) . . . . yes P(2) C(26) C(27) C(32) 7.7(6) . . . . yes P(2) C(26) C(31) C(30) 170.7(3) . . . . yes P(2) C(26) C(31) C(40) -10.0(6) . . . . yes N(1) Rh(1) P(1) C(1) -179.3(3) . . . . yes N(1) Rh(1) P(1) C(19) -2.0(2) . . . . yes N(1) Rh(1) P(2) C(25) 2.5(2) . . . . yes N(1) Rh(1) P(2) C(26) 179.6(3) . . . . yes N(1) C(20) C(21) C(22) -1.4(7) . . . . yes N(1) C(24) C(23) C(22) 0.5(7) . . . . yes C(1) P(1) C(19) C(20) 179.5(3) . . . . yes C(1) C(2) C(3) C(4) -1.5(6) . . . . yes C(1) C(2) C(7) C(8) -92.0(7) . . . . yes C(1) C(2) C(7) C(9) 33.0(7) . . . . yes C(1) C(2) C(7) C(10) 150.6(5) . . . . yes C(1) C(6) C(5) C(4) 3.4(6) . . . . yes C(1) C(6) C(15) C(16) -145.6(5) . . . . yes C(1) C(6) C(15) C(17) 97.3(5) . . . . yes C(1) C(6) C(15) C(18) -27.1(6) . . . . yes C(2) C(1) P(1) C(19) 92.5(4) . . . . yes C(2) C(1) C(6) C(5) -11.2(6) . . . . yes C(2) C(1) C(6) C(15) 168.0(4) . . . . yes C(2) C(3) C(4) C(5) -6.0(7) . . . . yes C(2) C(3) C(4) C(11) 176.2(4) . . . . yes C(3) C(2) C(1) C(6) 10.3(6) . . . . yes C(3) C(2) C(7) C(8) 88.7(7) . . . . yes C(3) C(2) C(7) C(9) -146.3(5) . . . . yes C(3) C(2) C(7) C(10) -28.7(6) . . . . yes C(3) C(4) C(5) C(6) 5.0(7) . . . . yes C(3) C(4) C(11) C(12) -11.5(7) . . . . yes C(3) C(4) C(11) C(13) 107.0(5) . . . . yes C(3) C(4) C(11) C(14) -133.4(5) . . . . yes C(4) C(3) C(2) C(7) 177.9(4) . . . . yes C(4) C(5) C(6) C(15) -175.8(4) . . . . yes C(5) C(4) C(11) C(12) 170.7(5) . . . . yes C(5) C(4) C(11) C(13) -70.7(6) . . . . yes C(5) C(4) C(11) C(14) 48.8(6) . . . . yes C(5) C(6) C(15) C(16) 33.6(6) . . . . yes C(5) C(6) C(15) C(17) -83.5(5) . . . . yes C(5) C(6) C(15) C(18) 152.1(4) . . . . yes C(6) C(1) P(1) C(19) -74.3(3) . . . . yes C(6) C(1) C(2) C(7) -169.0(4) . . . . yes C(6) C(5) C(4) C(11) -177.1(4) . . . . yes C(19) C(20) N(1) C(24) 179.3(4) . . . . yes C(19) C(20) C(21) C(22) 179.3(4) . . . . yes C(20) N(1) C(24) C(23) 0.5(6) . . . . yes C(20) N(1) C(24) C(25) -179.2(4) . . . . yes C(20) C(21) C(22) C(23) 2.3(7) . . . . yes C(21) C(20) N(1) C(24) 0.0(6) . . . . yes C(21) C(22) C(23) C(24) -1.9(7) . . . . yes C(22) C(23) C(24) C(25) -179.9(4) . . . . yes C(24) C(25) P(2) C(26) -179.7(3) . . . . yes C(25) P(2) C(26) C(27) 83.8(4) . . . . yes C(25) P(2) C(26) C(31) -91.0(4) . . . . yes C(26) C(27) C(28) C(29) -2.1(6) . . . . yes C(26) C(27) C(32) C(33) 154.5(4) . . . . yes C(26) C(27) C(32) C(34) -85.7(5) . . . . yes C(26) C(27) C(32) C(35) 36.2(6) . . . . yes C(26) C(31) C(30) C(29) 0.1(6) . . . . yes C(26) C(31) C(40) C(41) 79.3(6) . . . . yes C(26) C(31) C(40) C(42) -44.2(6) . . . . yes C(26) C(31) C(40) C(43) -162.6(5) . . . . yes C(27) C(26) C(31) C(30) -4.2(6) . . . . yes C(27) C(26) C(31) C(40) 175.1(4) . . . . yes C(27) C(28) C(29) C(30) -1.9(6) . . . . yes C(27) C(28) C(29) C(36) 180.0(4) . . . . yes C(28) C(27) C(26) C(31) 5.1(6) . . . . yes C(28) C(27) C(32) C(33) -28.0(5) . . . . yes C(28) C(27) C(32) C(34) 91.7(5) . . . . yes C(28) C(27) C(32) C(35) -146.4(4) . . . . yes C(28) C(29) C(30) C(31) 2.9(6) . . . . yes C(28) C(29) C(36) C(37) 0.8(6) . . . . yes C(28) C(29) C(36) C(38) -120.7(5) . . . . yes C(28) C(29) C(36) C(39) 120.3(5) . . . . yes C(29) C(28) C(27) C(32) -179.8(4) . . . . yes C(29) C(30) C(31) C(40) -179.2(4) . . . . yes C(30) C(29) C(36) C(37) -177.3(4) . . . . yes C(30) C(29) C(36) C(38) 61.2(6) . . . . yes C(30) C(29) C(36) C(39) -57.9(6) . . . . yes C(30) C(31) C(40) C(41) -101.4(5) . . . . yes C(30) C(31) C(40) C(42) 135.1(5) . . . . yes C(30) C(31) C(40) C(43) 16.7(6) . . . . yes C(31) C(26) C(27) C(32) -177.5(4) . . . . yes C(31) C(30) C(29) C(36) -178.9(4) . . . . yes C(44) O(1) C(46) C(47) 175(2) . . . . yes C(45) C(44) O(1) C(46) 170(2) . . . . yes C(48) O(2) C(50) C(51) 165.4(6) . . . . yes C(49) C(48) O(2) C(50) -171.3(6) . . . . yes C(49) C(48) O(2) C(50) -171.3(6) . . . . yes _chemical_name_common 'complex 1a' _exptl_crystal_recrystallization_method 'From Et2O at 203 K' _diffrn_ambient_temperature 296 #------------------------------------------------------------------------------ #------------------------------------------------------------------------------