# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1279 data_global # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in the Journal of the Chemical Society, Dalton Trans. ; _publ_contact_author 'Jean-Claude Daran' _publ_contact_author_address ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; _publ_contact_author_phone ' (33) 5 61 33 31 74 ' _publ_contact_author_fax ' (33) 5 61 55 30 03 ' _publ_contact_author_email ' daran@lcc-toulouse.fr ' _publ_requested_journal 'J. of Chem. Soc.,Dalton Trans.' #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; An unprecedented /K2-(N,H) bonding mode for a hydidotris(pyrazolyl) borato ligand ; loop_ _publ_author_name _publ_author_address 'Malbosc Francois ' ; Laboratoire de Catalyse, Chimie Fine et Polymeres, ENSCT, 118 Route de Narbonne, 31077 Toulouse Cedex 4, France ; 'Kalck Philippe' ; Laboratoire de Catalyse, Chimie Fine et Polymeres, ENSCT, 118 Route de Narbonne, 31077 Toulouse Cedex 4, France ; 'Daran Jean-Claude' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Etienne Michel' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; #======================================================================= _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435,435 Prince, E. Mathematical Techniques in Crystallography, Springer-Verlag: Berlin, 1982. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Revision 1.01. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #*********************************************************************** data_2a _chemical_name_systematic ; ? ; _chemical_formula_sum ' C29 H32 Rh1 CL3 B1 P1 O1 N6 ' _chemical_formula_moiety ' C29 H32 Rh1 CL3 B1 P1 O1 N6 ' _chemical_compound_source ; synthetic route ; _chemical_melting_point 'not measured' _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Rh ' -1.2870 0.9190 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International_Tables_Vol_IV_Table_2.2B' _cell_length_a 9.0263(14) _cell_length_b 10.4338(16) _cell_length_c 17.2896(24) _cell_angle_alpha 88.912(17) _cell_angle_beta 85.958(18) _cell_angle_gamma 77.907(18) _cell_volume 1556.8(3) _chemical_formula_weight 731.66 _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.2 _exptl_crystal_description box _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type 'numerical (X-Shape)' _exptl_absorpt_correction_T_min 0.8026 _exptl_absorpt_correction_T_max 0.9130 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 70 mm. 156 frames (3 min per frame) were obtained with 0 < \f < 249.6\% and with the crystals rotated through 1.6\% in \f. Coverage of the unique set was over 91.4% complete to at least 26.2\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '/f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% negligible _diffrn_reflns_number 15694 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.20 _reflns_number_total 5810 _reflns_number_gt 4794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al., 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _refine_ls_matrix_type full _refine_diff_density_min -0.52 _refine_diff_density_max 0.58 _refine_ls_number_reflns 4794 _refine_ls_number_parameters 384 _refine_ls_R_factor_obs 0.0237 _refine_ls_wR_factor_obs 0.0273 _refine_ls_goodness_of_fit_obs 1.0742 _refine_ls_shift/su_max 0.136428 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(1.22, -0.113, 0.953) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Rh1 1.001434(16) 0.290842(15) 0.718868(8) 0.0173 1.0000 Uani Cl1 1.31819(7) 0.26373(6) 1.00709(3) 0.0372 1.0000 Uani Cl2 1.51757(7) 0.29131(6) 0.49248(3) 0.0392 1.0000 Uani Cl3 0.90439(7) -0.22051(6) 0.62380(4) 0.0411 1.0000 Uani B1 1.2850(2) 0.0508(2) 0.73287(12) 0.0186 1.0000 Uani P1 0.77504(5) 0.29715(5) 0.78415(3) 0.0176 1.0000 Uani O1 0.8320(2) 0.3380(3) 0.57710(11) 0.0624 1.0000 Uani N1 1.13997(17) 0.24457(16) 0.81178(9) 0.0185 1.0000 Uani N2 1.25122(17) 0.13249(16) 0.80769(9) 0.0188 1.0000 Uani N3 1.21048(18) 0.25949(17) 0.65428(9) 0.0214 1.0000 Uani N4 1.31166(17) 0.14317(17) 0.66446(9) 0.0187 1.0000 Uani N5 1.0846(2) -0.06379(18) 0.7869(1) 0.0250 1.0000 Uani N6 1.14856(18) -0.01450(16) 0.72131(9) 0.0198 1.0000 Uani C1 0.8958(2) 0.3232(3) 0.63293(13) 0.0325 1.0000 Uani C11 1.1480(2) 0.3044(2) 0.87816(11) 0.0203 1.0000 Uani C12 1.2636(2) 0.2279(2) 0.91806(11) 0.0224 1.0000 Uani C13 1.3267(2) 0.1204(2) 0.87321(11) 0.0208 1.0000 Uani C14 1.0492(2) 0.4327(2) 0.90024(13) 0.0288 1.0000 Uani C15 1.4507(2) 0.0080(2) 0.89157(12) 0.0304 1.0000 Uani C31 1.2657(2) 0.3243(2) 0.59605(11) 0.0244 1.0000 Uani C32 1.4038(2) 0.2478(2) 0.56807(11) 0.0241 1.0000 Uani C33 1.4304(2) 0.1347(2) 0.61175(11) 0.0207 1.0000 Uani C34 1.1877(3) 0.4557(3) 0.56981(15) 0.0387 1.0000 Uani C35 1.5597(2) 0.0189(2) 0.60316(12) 0.0256 1.0000 Uani C51 0.9948(2) -0.1381(2) 0.76264(13) 0.0272 1.0000 Uani C52 1.0017(2) -0.1379(2) 0.68175(12) 0.0252 1.0000 Uani C53 1.1002(2) -0.0596(2) 0.65655(11) 0.0224 1.0000 Uani C54 0.9024(3) -0.2057(3) 0.81852(17) 0.0448 1.0000 Uani C55 1.1486(3) -0.0276(3) 0.57546(12) 0.0331 1.0000 Uani C111 0.7009(2) 0.1587(2) 0.75358(13) 0.0290 1.0000 Uani C121 0.6233(2) 0.4376(2) 0.76539(11) 0.0215 1.0000 Uani C122 0.6605(2) 0.5546(2) 0.74115(15) 0.0341 1.0000 Uani C123 0.5476(3) 0.6629(3) 0.72633(18) 0.0443 1.0000 Uani C124 0.3977(3) 0.6541(3) 0.73360(15) 0.0396 1.0000 Uani C125 0.3595(2) 0.5371(3) 0.75706(15) 0.0380 1.0000 Uani C126 0.4712(2) 0.4293(2) 0.77332(14) 0.0319 1.0000 Uani C131 0.7660(2) 0.2805(2) 0.88952(11) 0.0207 1.0000 Uani C132 0.8439(2) 0.1652(2) 0.92262(12) 0.0279 1.0000 Uani C133 0.8392(3) 0.1513(3) 1.00253(13) 0.0361 1.0000 Uani C134 0.7596(3) 0.2517(3) 1.05013(12) 0.0340 1.0000 Uani C135 0.6849(2) 0.3665(2) 1.01769(12) 0.0305 1.0000 Uani C136 0.6869(2) 0.3810(2) 0.93750(12) 0.0250 1.0000 Uani H1 1.388(3) -0.017(3) 0.7372(15) 0.032(6) 1.0000 Uiso H1111 0.7742 0.0787 0.7615 0.0354 1.0000 Uiso H1112 0.6083 0.1553 0.7837 0.0354 1.0000 Uiso H1113 0.6819 0.1676 0.6997 0.0354 1.0000 Uiso H141 0.9796 0.4610 0.8608 0.0348 1.0000 Uiso H142 1.1113 0.4962 0.9051 0.0348 1.0000 Uiso H143 0.9936 0.4243 0.9487 0.0348 1.0000 Uiso H151 1.4708 -0.0521 0.8489 0.0356 1.0000 Uiso H152 1.5410 0.0397 0.8997 0.0356 1.0000 Uiso H153 1.4207 -0.0355 0.9374 0.0356 1.0000 Uiso H341 1.0941 0.4832 0.6002 0.0440 1.0000 Uiso H342 1.2517 0.5173 0.5750 0.0440 1.0000 Uiso H343 1.1671 0.4511 0.5160 0.0440 1.0000 Uiso H351 1.6308 0.0351 0.5622 0.0297 1.0000 Uiso H352 1.6093 0.0045 0.6509 0.0297 1.0000 Uiso H353 1.5215 -0.0571 0.5912 0.0297 1.0000 Uiso H541 0.9223 -0.1873 0.8708 0.0547 1.0000 Uiso H542 0.9305 -0.2988 0.8101 0.0547 1.0000 Uiso H543 0.7969 -0.1756 0.8112 0.0547 1.0000 Uiso H551 1.0994 -0.0707 0.5398 0.0391 1.0000 Uiso H552 1.2569 -0.0560 0.5672 0.0391 1.0000 Uiso H553 1.1215 0.0658 0.5676 0.0391 1.0000 Uiso H1221 0.7650 0.5610 0.7345 0.0380 1.0000 Uiso H1231 0.5746 0.7441 0.7106 0.0463 1.0000 Uiso H1241 0.3198 0.7286 0.7226 0.0432 1.0000 Uiso H1251 0.2546 0.5312 0.7622 0.0403 1.0000 Uiso H1261 0.4436 0.3483 0.7896 0.0344 1.0000 Uiso H1321 0.9006 0.0959 0.8901 0.0328 1.0000 Uiso H1331 0.8914 0.0711 1.0252 0.0413 1.0000 Uiso H1341 0.7569 0.2413 1.1054 0.0381 1.0000 Uiso H1351 0.6311 0.4365 1.0504 0.0357 1.0000 Uiso H1361 0.6336 0.4608 0.9151 0.0290 1.0000 Uiso 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 0.01359(6) 0.02020(8) 0.01610(6) 0.00280(5) -0.00165(5) 0.00073(5) Cl1 0.0451(3) 0.0478(4) 0.0217(2) -0.0028(2) -0.0130(2) -0.0125(3) Cl2 0.0388(3) 0.0440(4) 0.0348(3) 0.0050(2) 0.0150(2) -0.0147(2) Cl3 0.0315(3) 0.0342(4) 0.0603(4) -0.0129(3) -0.0116(3) -0.0089(2) B1 0.018(1) 0.0169(12) 0.019(1) 0.0031(8) -0.0011(7) 0.0003(8) P1 0.0143(2) 0.0175(3) 0.0199(2) 0.00110(17) -0.00156(17) -0.00098(1) O1 0.0499(11) 0.1067(19) 0.033(1) 0.0272(11) -0.0225(9) -0.0183(11) N1 0.0145(7) 0.0200(9) 0.0197(7) -0.0009(6) 0.0003(6) -0.0007(6) N2 0.0163(7) 0.0193(9) 0.0194(7) 0.0038(6) -0.0008(6) -0.0011(6) N3 0.0209(8) 0.0207(9) 0.0200(8) 0.0052(6) -0.0017(6) 0.0012(6) N4 0.0163(7) 0.0198(9) 0.0182(7) 0.0013(6) -0.0013(6) 0.0004(6) N5 0.0279(8) 0.024(1) 0.0230(8) 0.0059(7) 0.0032(7) -0.0064(7) N6 0.0215(8) 0.0186(9) 0.0185(7) 0.0035(6) -0.0012(6) -0.0026(6) C1 0.023(1) 0.0456(15) 0.0260(11) 0.0091(9) 0.0005(8) -0.0023(9) C11 0.0190(9) 0.0245(11) 0.0187(9) -0.0020(7) 0.0007(7) -0.0083(7) C12 0.0224(9) 0.0316(12) 0.0160(8) 0.0020(7) -0.0031(7) -0.0113(8) C13 0.0190(9) 0.0280(11) 0.0171(8) 0.0079(7) -0.0026(7) -0.0089(8) C14 0.025(1) 0.0289(13) 0.0332(11) -0.0117(9) -0.0010(8) -0.0056(8) C15 0.0289(11) 0.0347(13) 0.026(1) 0.0103(9) -0.0090(8) -0.0013(9) C31 0.0231(9) 0.0276(12) 0.0222(9) 0.0065(8) 0.0001(7) -0.0061(8) C32 0.0238(9) 0.0287(12) 0.0208(9) 0.0008(8) 0.0031(7) -0.0097(8) C33 0.0193(9) 0.0246(12) 0.0190(9) -0.0037(7) -0.0017(7) -0.0058(8) C34 0.0364(12) 0.0325(14) 0.0434(13) 0.0176(11) 0.002(1) -0.002(1) C35 0.0206(9) 0.0256(12) 0.028(1) -0.0083(8) 0.0019(8) 0.0000(8) C51 0.025(1) 0.0184(12) 0.0371(11) 0.0024(8) 0.0001(8) -0.0024(8) C52 0.0203(9) 0.0172(11) 0.0370(11) -0.0038(8) -0.0047(8) 0.0002(7) C53 0.0190(9) 0.0205(11) 0.026(1) -0.0026(7) -0.0036(7) 0.0002(7) C54 0.0441(14) 0.0372(16) 0.0562(16) 0.0141(12) 0.0009(12) -0.0184(11) C55 0.0329(11) 0.0468(15) 0.022(1) -0.0048(9) -0.0036(8) -0.012(1) C111 0.0296(11) 0.0256(12) 0.0339(11) -0.0023(8) -0.0048(8) -0.0093(9) C121 0.0161(9) 0.0221(11) 0.0240(9) 0.0006(7) -0.0013(7) 0.0007(7) C122 0.022(1) 0.0248(13) 0.0543(14) 0.004(1) -0.0038(9) -0.0030(8) C123 0.0390(13) 0.0210(14) 0.0687(18) 0.0113(12) -0.0053(12) 0.003(1) C124 0.0307(12) 0.0344(15) 0.0448(13) 0.006(1) -0.003(1) 0.013(1) C125 0.018(1) 0.0458(16) 0.0453(13) 0.0057(11) -0.0019(9) 0.0038(9) C126 0.019(1) 0.0322(13) 0.0415(12) 0.009(1) 0.0003(8) -0.0003(8) C131 0.0170(8) 0.0230(11) 0.0223(9) -0.0004(7) -0.0015(7) -0.0046(7) C132 0.0300(11) 0.0255(12) 0.025(1) 0.0028(8) 0.0000(8) -0.0001(8) C133 0.0385(12) 0.0367(15) 0.0287(11) 0.0092(9) -0.0012(9) 0.001(1) C134 0.0320(11) 0.0494(16) 0.021(1) 0.0024(9) 0.0009(8) -0.010(1) C135 0.023(1) 0.0398(14) 0.028(1) -0.0091(9) 0.0041(8) -0.0043(9) C136 0.0194(9) 0.0266(12) 0.028(1) -0.0020(8) -0.0010(7) -0.0015(8) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rh1 . P1 . 2.2528(5) yes Rh1 . N1 . 2.0923(15) yes Rh1 . N3 . 2.0911(16) yes Rh1 . C1 . 1.810(2) yes Cl1 . C12 . 1.7198(19) yes Cl2 . C32 . 1.7183(19) yes Cl3 . C52 . 1.729(2) yes B1 . N2 . 1.539(3) yes B1 . N4 . 1.549(3) yes B1 . N6 . 1.553(3) yes B1 . H1 . 1.05(3) no P1 . C111 . 1.815(2) yes P1 . C121 . 1.8255(19) yes P1 . C131 . 1.8246(19) yes O1 . C1 . 1.150(3) yes N1 . N2 . 1.372(2) yes N1 . C11 . 1.330(2) yes N2 . C13 . 1.353(2) yes N3 . N4 . 1.374(2) yes N3 . C31 . 1.328(3) yes N4 . C33 . 1.346(3) yes N5 . N6 . 1.376(2) yes N5 . C51 . 1.326(3) yes N6 . C53 . 1.357(3) yes C11 . C12 . 1.391(3) yes C11 . C14 . 1.484(3) yes C12 . C13 . 1.374(3) yes C13 . C15 . 1.488(3) yes C31 . C32 . 1.392(3) yes C31 . C34 . 1.483(3) yes C32 . C33 . 1.376(3) yes C33 . C35 . 1.495(3) yes C51 . C52 . 1.396(3) yes C51 . C54 . 1.494(3) yes C52 . C53 . 1.373(3) yes C53 . C55 . 1.492(3) yes C121 . C122 . 1.382(3) yes C121 . C126 . 1.390(3) yes C122 . C123 . 1.387(3) yes C123 . C124 . 1.372(4) yes C124 . C125 . 1.382(4) yes C125 . C126 . 1.383(3) yes C131 . C132 . 1.395(3) yes C131 . C136 . 1.390(3) yes C132 . C133 . 1.385(3) yes C133 . C134 . 1.387(4) yes C134 . C135 . 1.375(3) yes C135 . C136 . 1.391(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Rh1 . N1 . 98.42(4) yes P1 . Rh1 . N3 . 172.36(5) yes N1 . Rh1 . N3 . 82.62(6) yes P1 . Rh1 . C1 . 86.06(7) yes N1 . Rh1 . C1 . 174.86(8) yes N3 . Rh1 . C1 . 92.61(8) yes N2 . B1 . N4 . 108.31(16) yes N2 . B1 . N6 . 108.75(15) yes N4 . B1 . N6 . 111.68(15) yes N2 . B1 . H1 . 108.5(14) no N4 . B1 . H1 . 106.2(14) no N6 . B1 . H1 . 113.3(14) no Rh1 . P1 . C111 . 108.17(7) yes Rh1 . P1 . C121 . 116.77(6) yes C111 . P1 . C121 . 103.2(1) yes Rh1 . P1 . C131 . 119.34(6) yes C111 . P1 . C131 . 102.9(1) yes C121 . P1 . C131 . 104.45(9) yes Rh1 . N1 . N2 . 118.53(11) yes Rh1 . N1 . C11 . 133.23(13) yes N2 . N1 . C11 . 108.22(15) yes B1 . N2 . N1 . 120.66(14) yes B1 . N2 . C13 . 129.79(16) yes N1 . N2 . C13 . 109.19(16) yes Rh1 . N3 . N4 . 118.20(12) yes Rh1 . N3 . C31 . 133.05(14) yes N4 . N3 . C31 . 108.29(16) yes B1 . N4 . N3 . 120.40(15) yes B1 . N4 . C33 . 130.10(17) yes N3 . N4 . C33 . 109.31(16) yes N6 . N5 . C51 . 106.31(17) yes B1 . N6 . N5 . 116.30(15) yes B1 . N6 . C53 . 131.10(16) yes N5 . N6 . C53 . 110.71(16) yes Rh1 . C1 . O1 . 176.8(2) yes N1 . C11 . C12 . 108.00(18) yes N1 . C11 . C14 . 123.04(17) yes C12 . C11 . C14 . 128.93(19) yes Cl1 . C12 . C11 . 125.69(17) yes Cl1 . C12 . C13 . 126.57(15) yes C11 . C12 . C13 . 107.74(17) yes N2 . C13 . C12 . 106.83(17) yes N2 . C13 . C15 . 124.90(19) yes C12 . C13 . C15 . 128.25(17) yes N3 . C31 . C32 . 107.83(18) yes N3 . C31 . C34 . 123.18(19) yes C32 . C31 . C34 . 128.99(19) yes Cl2 . C32 . C31 . 124.74(16) yes Cl2 . C32 . C33 . 127.48(16) yes C31 . C32 . C33 . 107.78(17) yes N4 . C33 . C32 . 106.79(17) yes N4 . C33 . C35 . 124.35(18) yes C32 . C33 . C35 . 128.82(18) yes N5 . C51 . C52 . 109.66(18) yes N5 . C51 . C54 . 121.5(2) yes C52 . C51 . C54 . 128.9(2) yes Cl3 . C52 . C51 . 126.59(17) yes Cl3 . C52 . C53 . 126.24(17) yes C51 . C52 . C53 . 107.17(18) yes N6 . C53 . C52 . 106.13(17) yes N6 . C53 . C55 . 125.06(19) yes C52 . C53 . C55 . 128.81(19) yes P1 . C121 . C122 . 119.21(15) yes P1 . C121 . C126 . 121.74(16) yes C122 . C121 . C126 . 119.04(18) yes C121 . C122 . C123 . 120.5(2) yes C122 . C123 . C124 . 120.3(2) yes C123 . C124 . C125 . 119.6(2) yes C124 . C125 . C126 . 120.4(2) yes C121 . C126 . C125 . 120.1(2) yes P1 . C131 . C132 . 118.96(15) yes P1 . C131 . C136 . 121.70(15) yes C132 . C131 . C136 . 119.31(18) yes C131 . C132 . C133 . 119.7(2) yes C132 . C133 . C134 . 120.7(2) yes C133 . C134 . C135 . 119.69(19) yes C134 . C135 . C136 . 120.2(2) yes C131 . C136 . C135 . 120.35(19) yes #==END #======================================================================= data_3a _chemical_name_systematic ; ? ; _chemical_formula_sum ' C42 H45 Rh1 P2 CL3 O1 N6 B1 ' _chemical_formula_moiety ' C42 H45 Rh1 P2 CL3 O1 N6 B1 ' _chemical_compound_source ; synthetic route ; _chemical_melting_point 'not measured' _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Rh ' -1.2870 0.9190 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International_Tables_Vol_IV_Table_2.2B' _cell_length_a 11.1644(19) _cell_length_b 12.0058(19) _cell_length_c 17.097(3) _cell_angle_alpha 101.073(18) _cell_angle_beta 102.282(19) _cell_angle_gamma 92.460(19) _cell_volume 2189.1(6) _chemical_formula_weight 931.88 _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 24.25 _exptl_crystal_description box _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method none _exptl_crystal_F_000 955 _exptl_absorpt_coefficient_mu 0.6785 _exptl_absorpt_correction_type 'empirical(DIFABS)' _exptl_absorpt_correction_T_min 0.3603 _exptl_absorpt_correction_T_max 0.7748 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 80 mm. 156 frames (3 min per frame) were obtained with 0 < \f < 249.6\% and with the crystals rotated through 1.6\% in \f. Coverage of the unique set was over 98% complete to at least 24.3\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '/f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% negligible _diffrn_reflns_number 17587 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.25 _reflns_number_total 6532 _reflns_number_gt 5120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al., 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _refine_ls_matrix_type full _refine_diff_density_min -0.462 _refine_diff_density_max 0.721 _refine_ls_number_reflns 5120 _refine_ls_number_parameters 510 _refine_ls_R_factor_obs 0.0407 _refine_ls_wR_factor_obs 0.0425 _refine_ls_goodness_of_fit_obs 1.0112 _refine_ls_shift/su_max 0.074031 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(2.34, -0.0136, 1.94) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle, but those attached to the methyl groups of the phosphines were refined with an equivalent isotropic thermal parameter. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Rh1 0.35456(2) 0.20438(2) 0.197947(16) 0.0266 1.0000 Uani P1 0.28719(7) 0.30953(7) 0.09843(5) 0.0271 1.0000 Uani P2 0.46333(7) 0.10504(7) 0.29057(5) 0.0277 1.0000 Uani Cl1 0.57322(8) 0.62537(7) 0.43455(6) 0.0430 1.0000 Uani Cl2 -0.0450(1) 0.23798(11) 0.53824(7) 0.0603 1.0000 Uani Cl3 -0.23776(7) 0.40353(9) 0.11851(6) 0.0458 1.0000 Uani O1 0.3072(3) -0.0066(2) 0.0706(2) 0.0645 1.0000 Uani N1 0.3928(2) 0.3556(2) 0.28813(16) 0.0257 1.0000 Uani N2 0.3055(2) 0.3950(2) 0.32971(16) 0.0252 1.0000 Uani N3 0.2122(3) 0.2195(3) 0.4163(2) 0.0381 1.0000 Uani N4 0.1405(2) 0.2948(2) 0.38112(18) 0.0304 1.0000 Uani N5 0.0773(2) 0.5018(2) 0.27145(18) 0.0307 1.0000 Uani N6 0.0786(2) 0.3856(2) 0.25704(17) 0.0280 1.0000 Uani B1 0.1771(3) 0.3246(3) 0.3050(2) 0.0292 1.0000 Uani C1 0.3271(3) 0.0757(3) 0.1201(2) 0.0405 1.0000 Uani C11 0.4939(3) 0.4281(3) 0.3180(2) 0.0298 1.0000 Uani C12 0.4707(3) 0.5136(3) 0.3779(2) 0.0297 1.0000 Uani C13 0.3516(3) 0.4913(3) 0.3850(2) 0.0290 1.0000 Uani C14 0.6078(3) 0.4104(3) 0.2864(3) 0.0415 1.0000 Uani C15 0.2824(3) 0.5554(3) 0.4418(2) 0.0386 1.0000 Uani C31 0.1605(3) 0.1920(3) 0.4739(2) 0.0388 1.0000 Uani C32 0.0556(3) 0.2500(3) 0.4757(2) 0.0382 1.0000 Uani C33 0.0437(3) 0.3142(3) 0.4172(2) 0.0323 1.0000 Uani C34 0.2148(4) 0.1116(4) 0.5254(3) 0.0614 1.0000 Uani C35 -0.0531(4) 0.3909(4) 0.3958(3) 0.0479 1.0000 Uani C51 -0.0291(3) 0.5233(3) 0.2265(2) 0.0322 1.0000 Uani C52 -0.0950(3) 0.4208(3) 0.1843(2) 0.0314 1.0000 Uani C53 -0.0255(3) 0.3344(3) 0.2032(2) 0.0286 1.0000 Uani C54 -0.0655(3) 0.6407(3) 0.2258(3) 0.0437 1.0000 Uani C55 -0.0528(3) 0.2092(3) 0.1748(3) 0.0430 1.0000 Uani C111 0.2940(3) 0.4618(3) 0.1377(2) 0.0371 1.0000 Uani C121 0.3834(3) 0.3020(3) 0.0236(2) 0.0315 1.0000 Uani C122 0.4881(3) 0.2438(3) 0.0319(2) 0.0351 1.0000 Uani C123 0.5618(3) 0.2404(3) -0.0251(3) 0.0422 1.0000 Uani C124 0.5309(3) 0.2959(3) -0.0889(3) 0.0473 1.0000 Uani C125 0.4263(4) 0.3545(4) -0.0972(3) 0.0524 1.0000 Uani C126 0.3533(3) 0.3569(3) -0.0412(2) 0.0431 1.0000 Uani C131 0.1341(3) 0.2730(3) 0.0308(2) 0.0305 1.0000 Uani C132 0.1047(3) 0.1645(3) -0.0165(2) 0.0411 1.0000 Uani C133 -0.0094(4) 0.1328(4) -0.0696(3) 0.0499 1.0000 Uani C134 -0.0957(3) 0.2114(4) -0.0759(3) 0.0480 1.0000 Uani C135 -0.0679(3) 0.3180(4) -0.0294(3) 0.0481 1.0000 Uani C136 0.0455(3) 0.3510(3) 0.0248(2) 0.0379 1.0000 Uani C211 0.5002(3) 0.1798(3) 0.3972(2) 0.0382 1.0000 Uani C221 0.6096(3) 0.0604(3) 0.2697(2) 0.0309 1.0000 Uani C222 0.7193(3) 0.0858(3) 0.3286(2) 0.0390 1.0000 Uani C223 0.8266(3) 0.0408(4) 0.3118(3) 0.0477 1.0000 Uani C224 0.8250(3) -0.0282(3) 0.2378(3) 0.0502 1.0000 Uani C225 0.7165(4) -0.0519(4) 0.1774(3) 0.0562 1.0000 Uani C226 0.6103(3) -0.0067(3) 0.1940(3) 0.0453 1.0000 Uani C231 0.3818(3) -0.0285(3) 0.2951(2) 0.0316 1.0000 Uani C232 0.4367(3) -0.1290(3) 0.2965(3) 0.0488 1.0000 Uani C233 0.3705(4) -0.2263(3) 0.3016(3) 0.0555 1.0000 Uani C234 0.2487(4) -0.2231(3) 0.3061(3) 0.0510 1.0000 Uani C235 0.1940(4) -0.1243(4) 0.3051(3) 0.0543 1.0000 Uani C236 0.2587(3) -0.0267(3) 0.2984(3) 0.0446 1.0000 Uani H1 0.191(3) 0.238(3) 0.264(2) 0.024(8) 1.0000 Uiso H1111 0.2749(3) 0.5025(3) 0.0951(2) 0.0500 1.0000 Uiso H1112 0.3802(3) 0.4893(3) 0.1685(2) 0.0500 1.0000 Uiso H1113 0.2393(3) 0.4730(3) 0.1723(2) 0.0500 1.0000 Uiso H2111 0.5511(3) 0.2500(3) 0.4046(2) 0.0500 1.0000 Uiso H2112 0.4167(3) 0.2035(3) 0.4186(2) 0.0500 1.0000 Uiso H2113 0.5475(3) 0.1340(3) 0.4355(2) 0.0500 1.0000 Uiso H141 0.6707 0.4705 0.3152 0.0481 1.0000 Uiso H142 0.6374 0.3384 0.2954 0.0481 1.0000 Uiso H143 0.5913 0.4101 0.2291 0.0481 1.0000 Uiso H151 0.3335 0.6207 0.4763 0.0443 1.0000 Uiso H152 0.2591 0.5070 0.4765 0.0443 1.0000 Uiso H153 0.2095 0.5800 0.4117 0.0443 1.0000 Uiso H341 0.1638 0.1032 0.5632 0.0779 1.0000 Uiso H342 0.2957 0.1421 0.5551 0.0779 1.0000 Uiso H343 0.2178 0.0395 0.4912 0.0779 1.0000 Uiso H351 -0.1101 0.3907 0.4301 0.0633 1.0000 Uiso H352 -0.0151 0.4674 0.4036 0.0633 1.0000 Uiso H353 -0.0946 0.3657 0.3396 0.0633 1.0000 Uiso H541 -0.1438 0.6382 0.1898 0.0494 1.0000 Uiso H542 -0.0688 0.6776 0.2804 0.0494 1.0000 Uiso H543 -0.0047 0.6831 0.2079 0.0494 1.0000 Uiso H551 -0.1316 0.1931 0.1374 0.0486 1.0000 Uiso H552 -0.0555 0.1757 0.2218 0.0486 1.0000 Uiso H553 0.0095 0.1781 0.1493 0.0486 1.0000 Uiso H1221 0.5115 0.2059 0.0770 0.0401 1.0000 Uiso H1231 0.6330 0.1985 -0.0206 0.0468 1.0000 Uiso H1241 0.5839 0.2957 -0.1261 0.0535 1.0000 Uiso H1251 0.4056 0.3919 -0.1424 0.0618 1.0000 Uiso H1261 0.2813 0.3988 -0.0475 0.0530 1.0000 Uiso H1321 0.1647 0.1092 -0.0130 0.0484 1.0000 Uiso H1331 -0.0291 0.0569 -0.1025 0.0577 1.0000 Uiso H1341 -0.1752 0.1905 -0.1115 0.0546 1.0000 Uiso H1351 -0.1282 0.3727 -0.0347 0.0569 1.0000 Uiso H1361 0.0615 0.4270 0.0580 0.0474 1.0000 Uiso H2221 0.7204 0.1340 0.3812 0.0479 1.0000 Uiso H2231 0.9028 0.0595 0.3517 0.0540 1.0000 Uiso H2241 0.8994 -0.0601 0.2282 0.0576 1.0000 Uiso H2251 0.7156 -0.0999 0.1257 0.0681 1.0000 Uiso H2261 0.5352 -0.0222 0.1524 0.0505 1.0000 Uiso H2321 0.5213 -0.1314 0.2944 0.0573 1.0000 Uiso H2331 0.4094 -0.2965 0.3021 0.0641 1.0000 Uiso H2341 0.2009 -0.2892 0.3106 0.0614 1.0000 Uiso H2351 0.1104 -0.1217 0.3094 0.0621 1.0000 Uiso H2361 0.2183 0.0417 0.2956 0.0498 1.0000 Uiso 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 0.03067(12) 0.02140(11) 0.02672(14) 0.0049(1) 0.00420(9) 0.00324(9) P1 0.0303(4) 0.0253(4) 0.0272(5) 0.0075(3) 0.0073(3) 0.0046(3) P2 0.0289(4) 0.0247(4) 0.0292(5) 0.0070(3) 0.0048(3) 0.0034(3) Cl1 0.0380(4) 0.0359(4) 0.0450(5) 0.0003(4) -0.0044(4) -0.0039(3) Cl2 0.0603(6) 0.0859(8) 0.0514(7) 0.0305(6) 0.0329(5) 0.0127(5) Cl3 0.0257(4) 0.0601(6) 0.0446(6) 0.0077(4) -0.0040(4) 0.0001(4) O1 0.079(2) 0.0357(16) 0.058(2) -0.0091(15) -0.0136(16) 0.0137(14) N1 0.0250(12) 0.0261(13) 0.0271(15) 0.0063(11) 0.007(1) 0.004(1) N2 0.0255(13) 0.0258(13) 0.0246(15) 0.0038(11) 0.007(1) 0.004(1) N3 0.0353(15) 0.0415(16) 0.0445(19) 0.0213(14) 0.0119(13) 0.0096(12) N4 0.0285(13) 0.0281(13) 0.0370(17) 0.0109(12) 0.0087(11) 0.004(1) N5 0.0275(13) 0.0269(13) 0.0364(17) 0.0078(12) 0.0034(11) 0.001(1) N6 0.0260(13) 0.0292(14) 0.0292(16) 0.0071(11) 0.0068(11) 0.000(1) B1 0.0274(17) 0.0267(17) 0.035(2) 0.0071(16) 0.0084(15) 0.0028(13) C1 0.050(2) 0.0286(18) 0.038(2) 0.0064(17) -0.0016(16) 0.0093(15) C11 0.0273(15) 0.0276(16) 0.035(2) 0.0098(14) 0.0048(13) 0.0033(12) C12 0.0303(16) 0.0263(16) 0.0287(19) 0.0042(14) 0.0002(13) -0.0001(12) C13 0.0309(16) 0.0288(16) 0.0261(18) 0.0055(13) 0.0030(13) 0.0076(12) C14 0.0338(18) 0.043(2) 0.048(2) 0.0034(17) 0.0156(16) 0.0021(15) C15 0.0366(18) 0.0419(19) 0.033(2) 0.0014(16) 0.0032(14) 0.0085(14) C31 0.0407(19) 0.0413(19) 0.038(2) 0.0158(17) 0.0092(15) 0.0019(15) C32 0.0370(18) 0.046(2) 0.033(2) 0.0097(16) 0.0116(15) -0.0024(15) C33 0.0298(16) 0.0381(18) 0.030(2) 0.0061(15) 0.0107(13) 0.0034(13) C34 0.066(3) 0.064(3) 0.068(3) 0.040(3) 0.020(2) 0.017(2) C35 0.046(2) 0.064(3) 0.047(3) 0.021(2) 0.0267(18) 0.0242(19) C51 0.0264(16) 0.0402(18) 0.032(2) 0.0125(15) 0.0060(13) 0.0032(13) C52 0.0228(15) 0.0422(18) 0.0280(19) 0.0074(15) 0.0030(13) 0.0015(13) C53 0.0251(15) 0.0344(17) 0.0265(19) 0.0067(14) 0.0075(12) -0.0039(12) C54 0.0390(19) 0.041(2) 0.048(2) 0.0108(17) 0.0003(16) 0.0073(15) C55 0.0386(19) 0.0345(19) 0.053(2) 0.0097(17) 0.0054(16) -0.0061(15) C111 0.0460(19) 0.0284(17) 0.038(2) 0.0109(15) 0.0094(15) 0.0048(14) C121 0.0284(16) 0.0325(17) 0.033(2) 0.0042(14) 0.0087(13) -0.0013(13) C122 0.0319(17) 0.0306(17) 0.039(2) 0.0008(15) 0.0056(14) 0.0010(13) C123 0.0315(18) 0.0342(18) 0.054(3) -0.0089(17) 0.0115(16) -0.0002(14) C124 0.040(2) 0.054(2) 0.046(3) -0.0023(19) 0.0207(17) -0.0101(17) C125 0.049(2) 0.070(3) 0.045(3) 0.022(2) 0.0174(18) -0.001(2) C126 0.0359(18) 0.057(2) 0.042(2) 0.0190(19) 0.0128(16) 0.0067(16) C131 0.0286(16) 0.0339(17) 0.0323(19) 0.0122(14) 0.0085(13) 0.0046(13) C132 0.0366(18) 0.0391(19) 0.045(2) 0.0040(16) 0.0051(15) 0.0101(15) C133 0.039(2) 0.055(2) 0.048(3) 0.0027(19) 0.0018(17) -0.0020(17) C134 0.0320(18) 0.066(3) 0.046(2) 0.018(2) 0.0038(16) -0.0037(17) C135 0.0312(18) 0.060(3) 0.060(3) 0.030(2) 0.0094(17) 0.0128(17) C136 0.0365(18) 0.0368(18) 0.045(2) 0.0155(16) 0.0124(15) 0.0082(14) C211 0.0381(18) 0.0406(19) 0.033(2) 0.0052(16) 0.0033(14) 0.0047(14) C221 0.0288(16) 0.0254(15) 0.040(2) 0.0106(14) 0.0075(14) 0.0028(12) C222 0.0370(18) 0.048(2) 0.032(2) 0.0105(16) 0.0066(15) 0.0065(15) C223 0.0282(18) 0.063(3) 0.057(3) 0.026(2) 0.0098(16) 0.0060(16) C224 0.037(2) 0.045(2) 0.077(3) 0.018(2) 0.024(2) 0.0111(16) C225 0.049(2) 0.053(2) 0.060(3) -0.014(2) 0.021(2) -0.0006(18) C226 0.0312(18) 0.049(2) 0.048(3) -0.0066(18) 0.0084(16) -0.0005(15) C231 0.0348(17) 0.0331(17) 0.0270(19) 0.0119(14) 0.0026(13) -0.0004(13) C232 0.042(2) 0.041(2) 0.069(3) 0.030(2) 0.0075(18) 0.0060(16) C233 0.054(2) 0.039(2) 0.079(3) 0.033(2) 0.008(2) 0.0058(18) C234 0.054(2) 0.044(2) 0.055(3) 0.024(2) 0.0025(19) -0.0108(18) C235 0.041(2) 0.051(2) 0.073(3) 0.019(2) 0.0143(19) -0.0039(17) C236 0.0364(19) 0.0352(19) 0.063(3) 0.0111(18) 0.0133(17) 0.0042(15) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rh1 . P1 . 2.3273(8) yes Rh1 . P2 . 2.3317(8) yes Rh1 . N1 . 2.105(3) yes Rh1 . C1 . 1.802(4) yes P1 . C111 . 1.815(3) yes P1 . C121 . 1.829(3) yes P1 . C131 . 1.830(3) yes P2 . C211 . 1.822(4) yes P2 . C221 . 1.825(3) yes P2 . C231 . 1.832(3) yes Cl1 . C12 . 1.716(3) yes Cl2 . C32 . 1.727(4) yes Cl3 . C52 . 1.723(3) yes O1 . C1 . 1.150(5) yes N1 . N2 . 1.373(4) yes N1 . C11 . 1.339(4) yes N2 . B1 . 1.565(4) yes N2 . C13 . 1.348(4) yes N3 . N4 . 1.373(4) yes N3 . C31 . 1.327(5) yes N4 . B1 . 1.543(5) yes N4 . C33 . 1.361(4) yes N5 . N6 . 1.371(4) yes N5 . C51 . 1.334(4) yes N6 . B1 . 1.528(4) yes N6 . C53 . 1.357(4) yes B1 . H1 . 1.17(3) no C11 . C12 . 1.380(5) yes C11 . C14 . 1.490(5) yes C12 . C13 . 1.380(5) yes C13 . C15 . 1.489(5) yes C31 . C32 . 1.391(5) yes C31 . C34 . 1.492(5) yes C32 . C33 . 1.364(5) yes C33 . C35 . 1.482(5) yes C51 . C52 . 1.389(5) yes C51 . C54 . 1.485(5) yes C52 . C53 . 1.368(5) yes C53 . C55 . 1.485(5) yes C121 . C122 . 1.384(5) yes C121 . C126 . 1.385(5) yes C122 . C123 . 1.400(5) yes C123 . C124 . 1.374(6) yes C124 . C125 . 1.384(6) yes C125 . C126 . 1.380(6) yes C131 . C132 . 1.381(5) yes C131 . C136 . 1.392(5) yes C132 . C133 . 1.387(5) yes C133 . C134 . 1.380(6) yes C134 . C135 . 1.355(6) yes C135 . C136 . 1.391(5) yes C221 . C222 . 1.389(5) yes C221 . C226 . 1.388(6) yes C222 . C223 . 1.397(5) yes C223 . C224 . 1.368(6) yes C224 . C225 . 1.393(6) yes C225 . C226 . 1.386(6) yes C231 . C232 . 1.379(5) yes C231 . C236 . 1.389(5) yes C232 . C233 . 1.382(5) yes C233 . C234 . 1.379(6) yes C234 . C235 . 1.359(6) yes C235 . C236 . 1.386(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Rh1 . P2 . 167.54(3) yes P1 . Rh1 . N1 . 89.97(7) yes P2 . Rh1 . N1 . 90.21(7) yes P1 . Rh1 . C1 . 89.93(11) yes P2 . Rh1 . C1 . 89.46(11) yes N1 . Rh1 . C1 . 178.01(14) yes Rh1 . P1 . C111 . 114.23(12) yes Rh1 . P1 . C121 . 112.92(11) yes C111 . P1 . C121 . 102.12(16) yes Rh1 . P1 . C131 . 119.7(1) yes C111 . P1 . C131 . 104.77(15) yes C121 . P1 . C131 . 100.87(15) yes Rh1 . P2 . C211 . 115.45(12) yes Rh1 . P2 . C221 . 114.92(11) yes C211 . P2 . C221 . 105.07(16) yes Rh1 . P2 . C231 . 114.3(1) yes C211 . P2 . C231 . 102.40(17) yes C221 . P2 . C231 . 103.15(15) yes Rh1 . N1 . N2 . 120.64(18) yes Rh1 . N1 . C11 . 132.2(2) yes N2 . N1 . C11 . 107.2(3) yes N1 . N2 . B1 . 117.0(2) yes N1 . N2 . C13 . 109.9(2) yes B1 . N2 . C13 . 133.1(3) yes N4 . N3 . C31 . 107.0(3) yes N3 . N4 . B1 . 114.4(3) yes N3 . N4 . C33 . 110.0(3) yes B1 . N4 . C33 . 135.0(3) yes N6 . N5 . C51 . 106.3(3) yes N5 . N6 . B1 . 123.1(3) yes N5 . N6 . C53 . 110.9(3) yes B1 . N6 . C53 . 125.5(3) yes N2 . B1 . N4 . 110.4(3) yes N2 . B1 . N6 . 111.8(3) yes N4 . B1 . N6 . 112.2(3) yes N2 . B1 . H1 . 105.5(15) no N4 . B1 . H1 . 106.6(16) no N6 . B1 . H1 . 110.0(16) no Rh1 . C1 . O1 . 178.7(4) yes N1 . C11 . C12 . 108.8(3) yes N1 . C11 . C14 . 121.4(3) yes C12 . C11 . C14 . 129.8(3) yes Cl1 . C12 . C11 . 125.9(2) yes Cl1 . C12 . C13 . 126.6(3) yes C11 . C12 . C13 . 107.5(3) yes N2 . C13 . C12 . 106.6(3) yes N2 . C13 . C15 . 124.1(3) yes C12 . C13 . C15 . 129.2(3) yes N3 . C31 . C32 . 108.9(3) yes N3 . C31 . C34 . 121.7(3) yes C32 . C31 . C34 . 129.4(4) yes Cl2 . C32 . C31 . 125.8(3) yes Cl2 . C32 . C33 . 126.2(3) yes C31 . C32 . C33 . 108.0(3) yes N4 . C33 . C32 . 106.1(3) yes N4 . C33 . C35 . 125.6(3) yes C32 . C33 . C35 . 128.2(3) yes N5 . C51 . C52 . 109.2(3) yes N5 . C51 . C54 . 122.7(3) yes C52 . C51 . C54 . 128.2(3) yes Cl3 . C52 . C51 . 126.8(3) yes Cl3 . C52 . C53 . 125.4(3) yes C51 . C52 . C53 . 107.8(3) yes N6 . C53 . C52 . 105.8(3) yes N6 . C53 . C55 . 124.4(3) yes C52 . C53 . C55 . 129.8(3) yes P1 . C121 . C122 . 120.7(3) yes P1 . C121 . C126 . 120.1(3) yes C122 . C121 . C126 . 119.2(3) yes C121 . C122 . C123 . 120.0(3) yes C122 . C123 . C124 . 120.0(3) yes C123 . C124 . C125 . 120.2(3) yes C124 . C125 . C126 . 119.6(4) yes C121 . C126 . C125 . 121.0(4) yes P1 . C131 . C132 . 119.2(2) yes P1 . C131 . C136 . 122.5(3) yes C132 . C131 . C136 . 118.3(3) yes C131 . C132 . C133 . 121.5(3) yes C132 . C133 . C134 . 119.5(4) yes C133 . C134 . C135 . 119.3(3) yes C134 . C135 . C136 . 122.0(3) yes C131 . C136 . C135 . 119.3(3) yes P2 . C221 . C222 . 122.2(3) yes P2 . C221 . C226 . 118.9(3) yes C222 . C221 . C226 . 118.8(3) yes C221 . C222 . C223 . 119.8(4) yes C222 . C223 . C224 . 120.7(4) yes C223 . C224 . C225 . 120.2(3) yes C224 . C225 . C226 . 119.0(4) yes C221 . C226 . C225 . 121.5(4) yes P2 . C231 . C232 . 123.5(3) yes P2 . C231 . C236 . 117.6(3) yes C232 . C231 . C236 . 118.9(3) yes C231 . C232 . C233 . 120.6(4) yes C232 . C233 . C234 . 120.0(4) yes C233 . C234 . C235 . 119.8(3) yes C234 . C235 . C236 . 120.7(4) yes C231 . C236 . C235 . 119.9(3) yes #==END