Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'S.T.H. Willems' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'J.C. Russcher' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'P.H.M. Budzelaar' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'B. de Bruin' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'R. de Gelder' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'J.M.M. Smits' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'A.W. Gal' ; Department of Inorganic Chemistry Nijmegen SON Research Center University of Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; _publ_contact_author_name 'Prof Anton W. Gal' _publ_contact_author_address ; Inorganic Chemistry University Of Nijmegen Toernooiveld 1 Nijmegen 6525 ED NETHERLANDS ; # 1. SUBMISSION DETAILS _publ_contact_author_phone '031 024 3652185' _publ_contact_author_fax '031 024 3553450' _publ_contact_author_email gal@sci.kun.nl _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ? #============================================================================== # 4. TEXT _publ_section_title ; Spontaneous disproportionation of rhodium(I) bisoxazolinates to rhodium(II) ; data_SAND1 _database_code_CSD 174014 _audit_creation_method 'SHELXL, adapted and expanded' _audit_creation_date 2001-10-30 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H50 N4 O4 Rh' _chemical_formula_weight 633.65 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.5080(4) _cell_length_b 10.9760(2) _cell_length_c 17.9908(3) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.2252(9) _cell_angle_gamma 90.000(5) _cell_volume 3113.58(11) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 17110 _cell_measurement_theta_min 1.180 _cell_measurement_theta_max 27.490 _exptl_crystal_description 'rough fragment' _exptl_crystal_colour 'dark brown-red' _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.28 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KappaCCD on rotating anode' _diffrn_measurement_method 'area detector \f and \w scan' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.000 _diffrn_reflns_number 17110 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10938 _reflns_number_gt 10348 _reflns_number_observed 10348 _reflns_threshold_expression >2sigma(I) _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius "Collect" program suite' _computing_cell_refinement ? _computing_data_reduction 'Nonius "DENZO SMN" program suite' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTON (Spek, 1993), PLATON (Spek, 1990, 1995) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.7031P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_Flack -0.024(17) _refine_ls_number_reflns 10938 _refine_ls_number_parameters 728 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0282 _refine_ls_R_factor_obs 0.0282 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_all 0.0792 _refine_ls_wR_factor_gt 0.0765 _refine_ls_wR_factor_obs 0.0765 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_shift/esd_mean 0.000 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 Rh1 Rh 0.249339(10) 0.182793(15) 0.556869(9) 0.01497(6) Uani 1 d . . . N1 N 0.25136(14) -0.0013(2) 0.54144(12) 0.0167(4) Uani 1 d . . . C2 C 0.31837(16) -0.0890(3) 0.58370(14) 0.0179(5) Uani 1 d . . . H2 H 0.3742 -0.0604 0.5792 0.022 Uiso 1 calc R . . C3 C 0.29242(18) -0.2040(3) 0.53414(15) 0.0255(6) Uani 1 d . . . H3A H 0.3222 -0.2090 0.4939 0.031 Uiso 1 calc R . . H3B H 0.3051 -0.2782 0.5668 0.031 Uiso 1 calc R . . O4 O 0.20220(13) -0.18946(18) 0.49918(11) 0.0257(4) Uani 1 d . . . C5 C 0.18586(18) -0.0673(2) 0.50109(15) 0.0192(5) Uani 1 d . . . C6 C 0.10377(18) -0.0301(3) 0.46277(15) 0.0232(6) Uani 1 d . . . H6 H 0.0636 -0.0888 0.4356 0.028 Uiso 1 calc R . . C7 C 0.07873(18) 0.0901(3) 0.46300(16) 0.0204(6) Uani 1 d . . . O8 O -0.00368(13) 0.1126(2) 0.42277(13) 0.0300(5) Uani 1 d . . . C9 C -0.0195(2) 0.2385(3) 0.4378(2) 0.0321(7) Uani 1 d . . . H9A H -0.0473 0.2449 0.4793 0.038 Uiso 1 calc R . . H9B H -0.0557 0.2785 0.3902 0.038 Uiso 1 calc R . . C10 C 0.06936(19) 0.2959(3) 0.46360(18) 0.0238(6) Uani 1 d . . . H10 H 0.0727 0.3532 0.5076 0.029 Uiso 1 calc R . . N11 N 0.12330(12) 0.1870(3) 0.49453(10) 0.0186(4) Uani 1 d . . . C12 C 0.32615(18) -0.1062(3) 0.67114(15) 0.0204(6) Uani 1 d . . . C13 C 0.3571(2) 0.0120(3) 0.71601(16) 0.0289(6) Uani 1 d . . . H13A H 0.3630 -0.0005 0.7713 0.043 Uiso 1 calc R . . H13B H 0.3159 0.0771 0.6955 0.043 Uiso 1 calc R . . H13C H 0.4121 0.0350 0.7099 0.043 Uiso 1 calc R . . C14 C 0.3936(2) -0.2036(3) 0.70356(16) 0.0307(7) Uani 1 d . . . H14A H 0.4465 -0.1801 0.6933 0.046 Uiso 1 calc R . . H14B H 0.3740 -0.2818 0.6784 0.046 Uiso 1 calc R . . H14C H 0.4034 -0.2112 0.7598 0.046 Uiso 1 calc R . . C15 C 0.2417(2) -0.1444(3) 0.68281(17) 0.0284(7) Uani 1 d . . . H15A H 0.2227 -0.2210 0.6551 0.043 Uiso 1 calc R . . H15B H 0.1992 -0.0809 0.6623 0.043 Uiso 1 calc R . . H15C H 0.2491 -0.1559 0.7384 0.043 Uiso 1 calc R . . C16 C 0.09305(19) 0.3660(3) 0.39829(17) 0.0318(7) Uani 1 d . . . C17 C 0.0931(2) 0.2815(4) 0.33011(17) 0.0406(8) Uani 1 d . . . H17A H 0.1059 0.3291 0.2889 0.061 Uiso 1 calc R . . H17B H 0.0371 0.2435 0.3096 0.061 Uiso 1 calc R . . H17C H 0.1362 0.2181 0.3483 0.061 Uiso 1 calc R . . C18 C 0.0269(2) 0.4689(3) 0.3693(2) 0.0479(9) Uani 1 d . . . H18A H 0.0204 0.5145 0.4140 0.072 Uiso 1 calc R . . H18B H -0.0278 0.4331 0.3404 0.072 Uiso 1 calc R . . H18C H 0.0461 0.5240 0.3352 0.072 Uiso 1 calc R . . C19 C 0.1795(2) 0.4270(3) 0.4299(2) 0.0418(9) Uani 1 d . . . H19A H 0.2228 0.3648 0.4510 0.063 Uiso 1 calc R . . H19B H 0.1779 0.4844 0.4712 0.063 Uiso 1 calc R . . H19C H 0.1932 0.4710 0.3878 0.063 Uiso 1 calc R . . N21 N 0.24936(15) 0.3382(2) 0.61996(12) 0.0219(5) Uani 1 d . . . C22 C 0.18253(19) 0.3840(3) 0.65307(16) 0.0249(6) Uani 1 d . . . H22 H 0.1267 0.3827 0.6116 0.030 Uiso 1 calc R . . C23 C 0.2108(3) 0.5156(3) 0.6704(2) 0.0455(10) Uani 1 d . . . H23A H 0.1842 0.5688 0.6254 0.055 Uiso 1 calc R . . H23B H 0.1960 0.5462 0.7165 0.055 Uiso 1 calc R . . O24 O 0.30022(19) 0.5109(2) 0.68506(15) 0.0474(7) Uani 1 d . . . C25 C 0.3167(2) 0.4078(3) 0.64826(18) 0.0327(7) Uani 1 d . . . C26 C 0.3998(2) 0.3911(4) 0.64918(19) 0.0403(9) Uani 1 d . . . H26 H 0.4415 0.4487 0.6753 0.048 Uiso 1 calc R . . C27 C 0.42380(18) 0.2923(3) 0.61302(16) 0.0285(7) Uani 1 d . . . O28 O 0.50735(14) 0.2843(3) 0.61701(13) 0.0406(6) Uani 1 d . . . C29 C 0.51668(17) 0.1682(4) 0.58208(17) 0.0368(8) Uani 1 d . . . H29A H 0.5351 0.1039 0.6222 0.044 Uiso 1 calc R . . H29B H 0.5583 0.1738 0.5524 0.044 Uiso 1 calc R . . C30 C 0.42769(17) 0.1422(3) 0.52813(16) 0.0237(6) Uani 1 d . . . H30 H 0.4165 0.0527 0.5284 0.028 Uiso 1 calc R . . N31 N 0.37535(13) 0.2060(2) 0.57055(11) 0.0204(5) Uani 1 d . . . C32 C 0.17449(19) 0.3120(3) 0.72446(16) 0.0272(6) Uani 1 d . . . C33 C 0.1372(2) 0.1859(4) 0.69733(16) 0.0385(7) Uani 1 d . . . H33A H 0.1742 0.1432 0.6722 0.058 Uiso 1 calc R . . H33B H 0.0806 0.1954 0.6602 0.058 Uiso 1 calc R . . H33C H 0.1330 0.1388 0.7423 0.058 Uiso 1 calc R . . C34 C 0.1112(2) 0.3785(4) 0.7581(2) 0.0457(9) Uani 1 d . . . H34A H 0.0593 0.3965 0.7162 0.069 Uiso 1 calc R . . H34B H 0.1365 0.4548 0.7826 0.069 Uiso 1 calc R . . H34C H 0.0975 0.3266 0.7971 0.069 Uiso 1 calc R . . C35 C 0.2594(2) 0.2989(3) 0.78781(17) 0.0391(8) Uani 1 d . . . H35A H 0.2517 0.2493 0.8305 0.059 Uiso 1 calc R . . H35B H 0.2804 0.3797 0.8076 0.059 Uiso 1 calc R . . H35C H 0.3005 0.2594 0.7660 0.059 Uiso 1 calc R . . C36 C 0.41277(16) 0.1846(4) 0.44249(13) 0.0239(5) Uani 1 d . . . C37 C 0.4290(2) 0.3210(3) 0.43801(19) 0.0347(8) Uani 1 d . . . H37A H 0.4191 0.3447 0.3835 0.052 Uiso 1 calc R . . H37B H 0.4878 0.3394 0.4676 0.052 Uiso 1 calc R . . H37C H 0.3904 0.3665 0.4600 0.052 Uiso 1 calc R . . C38 C 0.4732(2) 0.1119(3) 0.4084(2) 0.0377(8) Uani 1 d . . . H38A H 0.4628 0.1337 0.3536 0.057 Uiso 1 calc R . . H38B H 0.4633 0.0245 0.4126 0.057 Uiso 1 calc R . . H38C H 0.5321 0.1313 0.4374 0.057 Uiso 1 calc R . . C39 C 0.32158(19) 0.1545(3) 0.39521(16) 0.0315(8) Uani 1 d . . . H39A H 0.2821 0.1993 0.4165 0.047 Uiso 1 calc R . . H39B H 0.3118 0.0668 0.3981 0.047 Uiso 1 calc R . . H39C H 0.3124 0.1781 0.3408 0.047 Uiso 1 calc R . . Rh2 Rh 0.746256(10) 0.193227(16) -0.066751(9) 0.01660(7) Uani 1 d . . . N41 N 0.75445(14) 0.0133(2) -0.03401(12) 0.0182(4) Uani 1 d . . . C42 C 0.69263(18) -0.0860(3) -0.06767(15) 0.0223(6) Uani 1 d . . . H42 H 0.6355 -0.0609 -0.0646 0.027 Uiso 1 calc R . . C43 C 0.7264(2) -0.1888(3) -0.00851(17) 0.0332(7) Uani 1 d . . . H43A H 0.6956 -0.1909 0.0311 0.040 Uiso 1 calc R . . H43B H 0.7204 -0.2690 -0.0348 0.040 Uiso 1 calc R . . O44 O 0.81437(15) -0.1589(2) 0.02651(12) 0.0323(5) Uani 1 d . . . C45 C 0.82250(19) -0.0372(3) 0.01340(15) 0.0237(6) Uani 1 d . . . C46 C 0.90110(19) 0.0143(3) 0.04984(17) 0.0281(7) Uani 1 d . . . H46 H 0.9440 -0.0351 0.0831 0.034 Uiso 1 calc R . . C47 C 0.91897(18) 0.1345(3) 0.03942(15) 0.0265(7) Uani 1 d . . . O48 O 0.99882(12) 0.1750(3) 0.07847(11) 0.0374(5) Uani 1 d . . . C49 C 1.0053(2) 0.2962(3) 0.0509(2) 0.0393(8) Uani 1 d . . . H49A H 1.0337 0.2959 0.0095 0.047 Uiso 1 calc R . . H49B H 1.0375 0.3497 0.0938 0.047 Uiso 1 calc R . . C50 C 0.91282(18) 0.3387(3) 0.01874(17) 0.0256(6) Uani 1 d . . . H50 H 0.9066 0.3862 -0.0301 0.031 Uiso 1 calc R . . N51 N 0.86872(13) 0.2196(2) -0.00206(12) 0.0207(5) Uani 1 d . . . C52 C 0.68475(18) -0.1202(3) -0.15302(16) 0.0233(6) Uani 1 d . . . C53 C 0.6445(2) -0.0151(3) -0.20684(17) 0.0312(7) Uani 1 d . . . H53A H 0.6803 0.0575 -0.1926 0.047 Uiso 1 calc R . . H53B H 0.5882 0.0022 -0.2017 0.047 Uiso 1 calc R . . H53C H 0.6392 -0.0375 -0.2608 0.047 Uiso 1 calc R . . C54 C 0.6242(2) -0.2297(3) -0.17502(18) 0.0339(7) Uani 1 d . . . H54A H 0.5700 -0.2091 -0.1663 0.051 Uiso 1 calc R . . H54B H 0.6494 -0.2999 -0.1427 0.051 Uiso 1 calc R . . H54C H 0.6148 -0.2499 -0.2300 0.051 Uiso 1 calc R . . C55 C 0.7713(2) -0.1539(3) -0.16234(17) 0.0300(7) Uani 1 d . . . H55A H 0.7647 -0.1738 -0.2169 0.045 Uiso 1 calc R . . H55B H 0.7942 -0.2247 -0.1297 0.045 Uiso 1 calc R . . H55C H 0.8102 -0.0849 -0.1464 0.045 Uiso 1 calc R . . C56 C 0.8822(2) 0.4191(3) 0.07645(18) 0.0327(7) Uani 1 d . . . C57 C 0.8881(2) 0.3505(4) 0.15198(17) 0.0473(10) Uani 1 d . . . H57A H 0.9470 0.3253 0.1765 0.071 Uiso 1 calc R . . H57B H 0.8516 0.2783 0.1403 0.071 Uiso 1 calc R . . H57C H 0.8696 0.4039 0.1875 0.071 Uiso 1 calc R . . C58 C 0.9376(3) 0.5338(4) 0.0939(3) 0.0617(12) Uani 1 d . . . H58A H 0.9146 0.5908 0.1244 0.093 Uiso 1 calc R . . H58B H 0.9378 0.5725 0.0449 0.093 Uiso 1 calc R . . H58C H 0.9956 0.5114 0.1235 0.093 Uiso 1 calc R . . C59 C 0.7905(2) 0.4606(3) 0.0398(2) 0.0374(8) Uani 1 d . . . H59A H 0.7533 0.3892 0.0273 0.056 Uiso 1 calc R . . H59B H 0.7864 0.5065 -0.0079 0.056 Uiso 1 calc R . . H59C H 0.7731 0.5127 0.0766 0.056 Uiso 1 calc R . . N61 N 0.74418(17) 0.3365(2) -0.13947(13) 0.0274(5) Uani 1 d . . . C62 C 0.8092(2) 0.3690(3) -0.17728(16) 0.0318(7) Uani 1 d . . . H62 H 0.8658 0.3696 -0.1370 0.038 Uiso 1 calc R . . C63 C 0.7847(4) 0.4992(4) -0.2027(2) 0.0618(14) Uani 1 d . . . H63A H 0.8153 0.5578 -0.1623 0.074 Uiso 1 calc R . . H63B H 0.7972 0.5180 -0.2520 0.074 Uiso 1 calc R . . O64 O 0.6956(3) 0.5027(3) -0.21295(16) 0.0703(11) Uani 1 d . . . C65 C 0.6790(3) 0.4083(4) -0.16894(19) 0.0450(10) Uani 1 d . . . C66 C 0.5979(3) 0.4002(4) -0.16332(19) 0.0561(13) Uani 1 d . . . H66 H 0.5577 0.4612 -0.1869 0.067 Uiso 1 calc R . . C67 C 0.5735(2) 0.3055(4) -0.12418(17) 0.0393(9) Uani 1 d . . . O68 O 0.49045(17) 0.3055(3) -0.12678(14) 0.0569(8) Uani 1 d . . . C69 C 0.47733(18) 0.1904(5) -0.0937(2) 0.0584(13) Uani 1 d . . . H69A H 0.4557 0.1286 -0.1349 0.070 Uiso 1 calc R . . H69B H 0.4365 0.1988 -0.0634 0.070 Uiso 1 calc R . . C70 C 0.56576(17) 0.1547(3) -0.04050(17) 0.0317(7) Uani 1 d . . . H70 H 0.5729 0.0646 -0.0437 0.038 Uiso 1 calc R . . N71 N 0.61947(14) 0.2162(2) -0.08212(12) 0.0264(6) Uani 1 d . . . C72 C 0.81361(19) 0.2827(3) -0.24488(16) 0.0285(7) Uani 1 d . . . C73 C 0.8479(2) 0.1597(3) -0.21112(19) 0.0390(9) Uani 1 d . . . H73A H 0.8101 0.1245 -0.1839 0.058 Uiso 1 calc R . . H73B H 0.9046 0.1702 -0.1744 0.058 Uiso 1 calc R . . H73C H 0.8511 0.1051 -0.2533 0.058 Uiso 1 calc R . . C74 C 0.8757(3) 0.3368(4) -0.2847(2) 0.0546(11) Uani 1 d . . . H74A H 0.9286 0.3592 -0.2452 0.082 Uiso 1 calc R . . H74B H 0.8505 0.4095 -0.3143 0.082 Uiso 1 calc R . . H74C H 0.8877 0.2764 -0.3202 0.082 Uiso 1 calc R . . C75 C 0.7269(2) 0.2666(4) -0.30483(17) 0.0393(8) Uani 1 d . . . H75A H 0.7322 0.2128 -0.3466 0.059 Uiso 1 calc R . . H75B H 0.7053 0.3461 -0.3267 0.059 Uiso 1 calc R . . H75C H 0.6874 0.2304 -0.2797 0.059 Uiso 1 calc R . . C76 C 0.58223(17) 0.1909(4) 0.04633(15) 0.0283(6) Uani 1 d . . . C77 C 0.5672(2) 0.3270(3) 0.05384(18) 0.0331(7) Uani 1 d . . . H77A H 0.5794 0.3484 0.1090 0.050 Uiso 1 calc R . . H77B H 0.5079 0.3465 0.0264 0.050 Uiso 1 calc R . . H77C H 0.6045 0.3736 0.0310 0.050 Uiso 1 calc R . . C78 C 0.5220(3) 0.1171(4) 0.0795(3) 0.0495(10) Uani 1 d . . . H78A H 0.5318 0.1384 0.1343 0.074 Uiso 1 calc R . . H78B H 0.5325 0.0300 0.0751 0.074 Uiso 1 calc R . . H78C H 0.4632 0.1359 0.0502 0.074 Uiso 1 calc R . . C79 C 0.6729(2) 0.1582(3) 0.09352(16) 0.0326(8) Uani 1 d . . . H79A H 0.7130 0.2066 0.0752 0.049 Uiso 1 calc R . . H79B H 0.6828 0.0714 0.0870 0.049 Uiso 1 calc R . . H79C H 0.6809 0.1756 0.1487 0.049 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01242(9) 0.01479(14) 0.01662(8) 0.00026(10) 0.00262(6) -0.00116(9) N1 0.0183(11) 0.0150(12) 0.0159(9) 0.0008(8) 0.0035(8) 0.0024(9) C2 0.0171(12) 0.0179(13) 0.0190(11) 0.0011(10) 0.0057(9) 0.0017(11) C3 0.0280(15) 0.0211(14) 0.0257(13) -0.0046(11) 0.0053(11) 0.0042(12) O4 0.0267(10) 0.0152(10) 0.0301(10) -0.0061(8) 0.0005(8) -0.0014(9) C5 0.0241(13) 0.0166(14) 0.0159(11) -0.0021(9) 0.0043(10) -0.0015(11) C6 0.0169(12) 0.0254(16) 0.0228(13) -0.0073(11) -0.0010(10) -0.0061(12) C7 0.0145(13) 0.0279(16) 0.0173(13) -0.0019(11) 0.0024(11) 0.0021(12) O8 0.0159(10) 0.0324(13) 0.0351(12) -0.0054(9) -0.0026(8) 0.0007(9) C9 0.0190(14) 0.0319(17) 0.0407(17) -0.0022(13) 0.0019(12) 0.0069(14) C10 0.0183(14) 0.0253(16) 0.0254(15) 0.0016(12) 0.0026(12) 0.0071(13) N11 0.0151(9) 0.0220(11) 0.0176(8) -0.0012(11) 0.0030(7) 0.0015(11) C12 0.0213(13) 0.0180(15) 0.0206(13) 0.0033(11) 0.0041(10) 0.0018(12) C13 0.0371(17) 0.0233(16) 0.0210(13) 0.0004(11) 0.0006(11) -0.0001(14) C14 0.0317(16) 0.0295(17) 0.0266(13) 0.0083(12) 0.0018(12) 0.0081(14) C15 0.0308(17) 0.0289(17) 0.0290(14) 0.0051(12) 0.0142(13) 0.0030(14) C16 0.0279(15) 0.0357(18) 0.0291(14) 0.0157(13) 0.0042(12) 0.0136(14) C17 0.0331(17) 0.062(2) 0.0249(14) 0.0095(15) 0.0063(12) 0.0174(17) C18 0.042(2) 0.046(2) 0.051(2) 0.0222(17) 0.0061(16) 0.0207(18) C19 0.0397(19) 0.037(2) 0.049(2) 0.0232(16) 0.0129(16) 0.0071(17) N21 0.0239(12) 0.0170(12) 0.0254(11) -0.0027(9) 0.0080(9) -0.0043(10) C22 0.0264(14) 0.0194(15) 0.0286(13) -0.0057(11) 0.0075(11) 0.0024(12) C23 0.066(3) 0.0250(19) 0.055(2) -0.0091(16) 0.032(2) -0.0039(19) O24 0.0629(18) 0.0286(14) 0.0599(16) -0.0221(12) 0.0321(14) -0.0225(13) C25 0.0420(19) 0.0270(17) 0.0333(16) -0.0098(14) 0.0177(14) -0.0155(16) C26 0.0367(18) 0.050(2) 0.0373(17) -0.0207(16) 0.0157(14) -0.0292(18) C27 0.0184(13) 0.0401(19) 0.0260(13) -0.0002(13) 0.0050(11) -0.0119(14) O28 0.0182(10) 0.0656(18) 0.0364(11) -0.0070(12) 0.0058(9) -0.0150(12) C29 0.0152(11) 0.056(2) 0.0379(14) 0.0093(17) 0.0064(10) 0.0052(17) C30 0.0172(12) 0.0266(15) 0.0288(13) 0.0094(11) 0.0091(10) 0.0033(11) N31 0.0152(9) 0.0251(15) 0.0202(9) 0.0033(9) 0.0041(7) -0.0015(10) C32 0.0277(15) 0.0316(17) 0.0248(13) -0.0095(12) 0.0116(11) -0.0039(13) C33 0.0443(17) 0.0396(19) 0.0376(14) -0.0096(18) 0.0215(12) -0.015(2) C34 0.0407(19) 0.055(2) 0.050(2) -0.0144(18) 0.0270(16) -0.0004(19) C35 0.0425(19) 0.048(2) 0.0232(14) -0.0052(14) 0.0034(13) -0.0012(17) C36 0.0234(12) 0.0241(14) 0.0260(11) 0.0048(15) 0.0102(9) 0.0014(17) C37 0.050(2) 0.0258(18) 0.0332(15) 0.0081(13) 0.0197(15) 0.0016(16) C38 0.0389(19) 0.040(2) 0.0425(18) 0.0072(15) 0.0251(16) 0.0069(16) C39 0.0273(14) 0.045(2) 0.0223(12) -0.0017(12) 0.0073(10) -0.0017(14) Rh2 0.01540(9) 0.01712(15) 0.01498(8) -0.00057(11) 0.00095(6) 0.00196(10) N41 0.0198(11) 0.0183(12) 0.0157(10) 0.0003(8) 0.0042(8) 0.0002(10) C42 0.0238(14) 0.0177(13) 0.0274(13) 0.0010(11) 0.0108(11) -0.0005(12) C43 0.0407(18) 0.0266(17) 0.0307(14) 0.0054(12) 0.0078(13) -0.0041(15) O44 0.0375(12) 0.0199(11) 0.0348(11) 0.0111(9) 0.0034(9) 0.0060(10) C45 0.0278(14) 0.0230(15) 0.0196(12) 0.0025(11) 0.0058(11) 0.0058(13) C46 0.0239(15) 0.0293(17) 0.0249(14) 0.0087(13) -0.0023(11) 0.0090(14) C47 0.0169(13) 0.0398(18) 0.0192(12) 0.0005(11) -0.0002(10) 0.0004(13) O48 0.0184(9) 0.0460(15) 0.0381(10) 0.0083(12) -0.0064(7) -0.0037(12) C49 0.0232(16) 0.046(2) 0.0459(18) -0.0011(16) 0.0059(14) -0.0124(16) C50 0.0209(14) 0.0289(17) 0.0245(14) -0.0012(12) 0.0027(11) -0.0073(13) N51 0.0150(10) 0.0253(15) 0.0195(9) 0.0001(8) 0.0013(8) -0.0030(9) C52 0.0218(13) 0.0216(16) 0.0257(13) -0.0067(11) 0.0056(10) -0.0027(12) C53 0.0306(16) 0.0291(17) 0.0252(14) -0.0028(12) -0.0048(12) 0.0021(14) C54 0.0314(16) 0.0285(17) 0.0397(16) -0.0110(13) 0.0073(13) -0.0078(14) C55 0.0260(15) 0.0333(18) 0.0319(14) -0.0085(13) 0.0103(12) -0.0016(14) C56 0.0303(16) 0.0324(18) 0.0327(15) -0.0131(13) 0.0048(13) -0.0121(14) C57 0.045(2) 0.069(3) 0.0248(15) -0.0133(16) 0.0051(14) -0.005(2) C58 0.058(3) 0.050(3) 0.082(3) -0.037(2) 0.028(2) -0.030(2) C59 0.0427(19) 0.0289(18) 0.0394(18) -0.0124(14) 0.0102(15) -0.0021(16) N61 0.0394(14) 0.0227(13) 0.0195(10) 0.0043(9) 0.0078(10) 0.0103(12) C62 0.0461(19) 0.0261(17) 0.0221(13) 0.0063(12) 0.0084(13) -0.0039(15) C63 0.119(4) 0.024(2) 0.051(2) 0.0093(17) 0.038(3) 0.007(2) O64 0.129(3) 0.0426(17) 0.0541(16) 0.0314(14) 0.0492(19) 0.054(2) C65 0.075(3) 0.038(2) 0.0279(17) 0.0132(15) 0.0234(17) 0.033(2) C66 0.069(3) 0.077(3) 0.0243(15) 0.0181(17) 0.0165(17) 0.057(3) C67 0.0296(16) 0.065(3) 0.0196(13) -0.0075(15) 0.0018(12) 0.0261(17) O68 0.0305(13) 0.100(3) 0.0356(12) -0.0101(15) 0.0021(10) 0.0296(16) C69 0.0143(12) 0.099(4) 0.059(2) -0.051(3) 0.0062(13) -0.006(2) C70 0.0178(12) 0.037(2) 0.0432(15) -0.0246(14) 0.0130(11) -0.0044(13) N71 0.0188(10) 0.0363(18) 0.0198(9) -0.0121(10) -0.0008(8) 0.0056(11) C72 0.0275(15) 0.0338(18) 0.0249(13) 0.0084(12) 0.0089(12) 0.0011(14) C73 0.0392(17) 0.044(3) 0.0387(15) 0.0076(15) 0.0191(13) 0.0139(17) C74 0.057(2) 0.064(3) 0.053(2) 0.013(2) 0.0329(19) -0.009(2) C75 0.0413(19) 0.050(2) 0.0223(14) -0.0004(14) 0.0028(13) 0.0072(17) C76 0.0319(13) 0.0236(15) 0.0351(12) -0.0107(16) 0.0185(10) -0.0050(18) C77 0.0453(19) 0.0287(18) 0.0292(15) -0.0093(13) 0.0172(14) -0.0005(16) C78 0.053(2) 0.041(2) 0.073(3) -0.0162(19) 0.046(2) -0.0155(19) C79 0.0404(17) 0.033(2) 0.0283(13) 0.0010(12) 0.0166(12) 0.0028(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N31 2.037(2) . Y Rh1 N1 2.041(2) . Y Rh1 N21 2.049(2) . Y Rh1 N11 2.0511(18) . Y N1 C5 1.325(4) . Y N1 C2 1.494(3) . Y C2 C3 1.531(4) . Y C2 C12 1.551(3) . Y C3 O4 1.444(3) . Y O4 C5 1.370(3) . Y C5 C6 1.388(4) . Y C6 C7 1.383(4) . Y C7 N11 1.321(4) . Y C7 O8 1.361(4) . Y O8 C9 1.447(4) . Y C9 C10 1.536(4) . Y C10 N11 1.496(4) . Y C10 C16 1.549(4) . Y C12 C14 1.529(4) . Y C12 C15 1.529(4) . Y C12 C13 1.533(4) . Y C16 C19 1.525(5) . Y C16 C17 1.538(5) . Y C16 C18 1.550(4) . Y N21 C25 1.321(4) . Y N21 C22 1.488(3) . Y C22 C23 1.522(5) . Y C22 C32 1.547(4) . Y C23 O24 1.421(5) . Y O24 C25 1.379(4) . Y C25 C26 1.379(5) . Y C26 C27 1.381(5) . Y C27 N31 1.327(4) . Y C27 O28 1.363(4) . Y O28 C29 1.449(5) . Y C29 C30 1.529(4) . Y C30 N31 1.487(3) . Y C30 C36 1.558(3) . Y C32 C35 1.529(4) . Y C32 C33 1.534(5) . Y C32 C34 1.538(4) . Y C36 C37 1.527(5) . Y C36 C39 1.530(4) . Y C36 C38 1.540(4) . Y Rh2 N51 2.033(2) . Y Rh2 N61 2.039(2) . Y Rh2 N71 2.044(2) . Y Rh2 N41 2.054(2) . Y N41 C45 1.315(4) . Y N41 C42 1.493(4) . Y C42 C43 1.538(4) . Y C42 C52 1.548(4) . Y C43 O44 1.439(4) . Y O44 C45 1.370(4) . Y C45 C46 1.389(4) . Y C46 C47 1.377(4) . Y C47 N51 1.323(4) . Y C47 O48 1.371(3) . Y O48 C49 1.435(4) . Y C49 C50 1.537(4) . Y C50 N51 1.490(4) . Y C50 C56 1.556(4) . Y C52 C53 1.526(4) . Y C52 C55 1.532(4) . Y C52 C54 1.538(4) . Y C56 C59 1.530(5) . Y C56 C57 1.531(5) . Y C56 C58 1.533(5) . Y N61 C65 1.312(4) . Y N61 C62 1.474(4) . Y C62 C63 1.518(5) . Y C62 C72 1.560(4) . Y C63 O64 1.427(6) . Y O64 C65 1.381(5) . Y C65 C66 1.375(6) . Y C66 C67 1.381(6) . Y C67 N71 1.330(4) . Y C67 O68 1.358(4) . Y O68 C69 1.440(6) . Y C69 C70 1.541(4) . Y C70 N71 1.482(4) . Y C70 C76 1.556(4) . Y C72 C73 1.519(5) . Y C72 C75 1.527(4) . Y C72 C74 1.534(4) . Y C76 C77 1.527(5) . Y C76 C79 1.528(4) . Y C76 C78 1.533(4) . Y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Rh1 N1 94.75(9) . . Y N31 Rh1 N21 89.80(10) . . Y N1 Rh1 N21 154.44(9) . . Y N31 Rh1 N11 153.84(8) . . Y N1 Rh1 N11 90.14(10) . . Y N21 Rh1 N11 96.78(10) . . Y C5 N1 C2 106.7(2) . . Y C5 N1 Rh1 124.89(19) . . Y C2 N1 Rh1 127.47(17) . . Y N1 C2 C3 101.4(2) . . Y N1 C2 C12 114.9(2) . . Y C3 C2 C12 114.5(2) . . Y O4 C3 C2 103.7(2) . . Y C5 O4 C3 106.4(2) . . Y N1 C5 O4 114.4(2) . . Y N1 C5 C6 129.0(3) . . Y O4 C5 C6 116.5(3) . . Y C7 C6 C5 121.9(3) . . Y N11 C7 O8 115.1(3) . . Y N11 C7 C6 129.8(3) . . Y O8 C7 C6 115.1(3) . . Y C7 O8 C9 106.3(2) . . Y O8 C9 C10 103.9(2) . . Y N11 C10 C9 101.2(2) . . Y N11 C10 C16 115.0(2) . . Y C9 C10 C16 114.0(3) . . Y C7 N11 C10 106.77(19) . . Y C7 N11 Rh1 124.2(2) . . Y C10 N11 Rh1 128.1(2) . . Y C14 C12 C15 110.2(3) . . Y C14 C12 C13 107.4(2) . . Y C15 C12 C13 109.6(2) . . Y C14 C12 C2 107.7(2) . . Y C15 C12 C2 111.6(2) . . Y C13 C12 C2 110.2(2) . . Y C19 C16 C17 109.9(3) . . Y C19 C16 C10 110.7(2) . . Y C17 C16 C10 111.4(3) . . Y C19 C16 C18 107.1(3) . . Y C17 C16 C18 109.7(3) . . Y C10 C16 C18 107.8(3) . . Y C25 N21 C22 106.8(2) . . Y C25 N21 Rh1 123.8(2) . . Y C22 N21 Rh1 128.67(19) . . Y N21 C22 C23 100.6(2) . . Y N21 C22 C32 114.6(2) . . Y C23 C22 C32 114.3(2) . . Y O24 C23 C22 104.0(3) . . Y C25 O24 C23 106.4(3) . . Y N21 C25 O24 113.3(3) . . Y N21 C25 C26 130.4(3) . . Y O24 C25 C26 116.2(3) . . Y C25 C26 C27 121.4(3) . . Y N31 C27 O28 114.3(3) . . Y N31 C27 C26 128.6(3) . . Y O28 C27 C26 116.9(3) . . Y C27 O28 C29 105.7(2) . . Y O28 C29 C30 103.5(2) . . Y N31 C30 C29 100.5(2) . . Y N31 C30 C36 114.9(2) . . Y C29 C30 C36 114.4(2) . . Y C27 N31 C30 106.8(2) . . Y C27 N31 Rh1 125.4(2) . . Y C30 N31 Rh1 127.38(18) . . Y C35 C32 C33 110.2(3) . . Y C35 C32 C34 109.3(3) . . Y C33 C32 C34 107.3(3) . . Y C35 C32 C22 112.4(3) . . Y C33 C32 C22 108.8(2) . . Y C34 C32 C22 108.7(3) . . Y C37 C36 C39 109.9(3) . . Y C37 C36 C38 110.0(2) . . Y C39 C36 C38 108.3(3) . . Y C37 C36 C30 111.5(3) . . Y C39 C36 C30 109.1(2) . . Y C38 C36 C30 107.9(3) . . Y N51 Rh2 N61 94.74(10) . . Y N51 Rh2 N71 149.87(9) . . Y N61 Rh2 N71 89.77(11) . . Y N51 Rh2 N41 90.15(9) . . Y N61 Rh2 N41 155.87(9) . . Y N71 Rh2 N41 97.78(10) . . Y C45 N41 C42 107.8(2) . . Y C45 N41 Rh2 124.2(2) . . Y C42 N41 Rh2 127.33(17) . . Y N41 C42 C43 101.0(2) . . Y N41 C42 C52 115.2(2) . . Y C43 C42 C52 114.5(2) . . Y O44 C43 C42 104.3(2) . . Y C45 O44 C43 106.5(2) . . Y N41 C45 O44 114.4(3) . . Y N41 C45 C46 129.4(3) . . Y O44 C45 C46 116.2(3) . . Y C47 C46 C45 122.2(3) . . Y N51 C47 O48 114.1(3) . . Y N51 C47 C46 129.0(3) . . Y O48 C47 C46 116.9(3) . . Y C47 O48 C49 106.4(2) . . Y O48 C49 C50 104.1(2) . . Y N51 C50 C49 100.7(2) . . Y N51 C50 C56 115.7(2) . . Y C49 C50 C56 113.8(3) . . Y C47 N51 C50 107.4(2) . . Y C47 N51 Rh2 125.0(2) . . Y C50 N51 Rh2 126.71(17) . . Y C53 C52 C55 111.0(3) . . Y C53 C52 C54 107.5(2) . . Y C55 C52 C54 109.8(3) . . Y C53 C52 C42 109.8(2) . . Y C55 C52 C42 111.1(2) . . Y C54 C52 C42 107.6(2) . . Y C59 C56 C57 108.9(3) . . Y C59 C56 C58 107.3(3) . . Y C57 C56 C58 110.2(3) . . Y C59 C56 C50 110.9(2) . . Y C57 C56 C50 111.4(3) . . Y C58 C56 C50 108.1(3) . . Y C65 N61 C62 106.9(3) . . Y C65 N61 Rh2 125.3(2) . . Y C62 N61 Rh2 127.3(2) . . Y N61 C62 C63 101.6(3) . . Y N61 C62 C72 114.9(3) . . Y C63 C62 C72 114.0(3) . . Y O64 C63 C62 103.7(3) . . Y C65 O64 C63 106.2(3) . . Y N61 C65 C66 129.2(4) . . Y N61 C65 O64 113.8(4) . . Y C66 C65 O64 117.0(3) . . Y C65 C66 C67 121.5(3) . . Y N71 C67 O68 114.8(4) . . Y N71 C67 C66 129.9(3) . . Y O68 C67 C66 115.2(3) . . Y C67 O68 C69 105.0(3) . . Y O68 C69 C70 104.4(3) . . Y N71 C70 C69 99.7(3) . . Y N71 C70 C76 116.0(2) . . Y C69 C70 C76 114.3(2) . . Y C67 N71 C70 107.3(3) . . Y C67 N71 Rh2 123.8(2) . . Y C70 N71 Rh2 128.12(19) . . Y C73 C72 C75 109.9(3) . . Y C73 C72 C74 108.0(3) . . Y C75 C72 C74 109.4(3) . . Y C73 C72 C62 109.0(2) . . Y C75 C72 C62 111.7(3) . . Y C74 C72 C62 108.8(3) . . Y C77 C76 C79 109.8(3) . . Y C77 C76 C78 109.9(3) . . Y C79 C76 C78 107.5(3) . . Y C77 C76 C70 110.7(3) . . Y C79 C76 C70 110.4(2) . . Y C78 C76 C70 108.4(3) . . Y _diffrn_reflns_theta_full 27.49 _refine_diff_density_max 0.555 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.065 _publ_section_experimental ; Crystal colour: dark brown-red, crystal shape: rough fragment. Special remarks: CCD Utrecht. Special experimental condition: crystal was mounted in a glass capillary. Special experimental condition: measurements were performed at -120 degrees C. Least-squares refinement using calculated weights: w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.7031P] where P=(Fo^2^+2Fc^2^)/3 ; #===END data_JAAP01 _database_code_CSD 174015 #============================================================================== _audit_creation_method 'SHELXL, adapted and expanded' _audit_creation_date 2001-10-31 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 N2 O2 Rh' _chemical_formula_weight 464.36 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.9724(7) _cell_length_b 11.7974(9) _cell_length_c 19.1120(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2023.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.196 _cell_measurement_theta_max 14.742 _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour 'red-brown transparant' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type experimental #_exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 1.478 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius CAD4' _diffrn_measurement_method \w/2\q-scan _diffrn_special_details ; \w/2\q-scan with variable scan width, variable scan speed and variable aperture. Scan width (0.48 + 0.61tan\q)\%, range: 0.76\%-1.19\%, aperture (1.30 + 0.80tan\q)mm., range: 1.34-1.71mm. Maximum scan time: 30 sec/reflection. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_time 6962 _diffrn_standards_decay_% 1.721 _diffrn_reflns_number 2635 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2635 _reflns_number_gt 2216 _reflns_number_observed 2216 _reflns_threshold_expression >2sigma(I) _reflns_observed_criterion >2sigma(I) _computing_data_collection ; CAD4 EXPRESS (Enraf-Nonius, 1994) ; #_computing_cell_refinement #; #CAD4 EXPRESS (Enraf-Nonius, 1994) #; _computing_data_reduction ; local programs (Smits et al., 1988), profile analysis (Lehman & Larsen, 1974, Grant & Gabe, 1978), EMPABS (North et al., 1968) ; _computing_structure_solution ; DIRDIF (Beurskens et al., 1996), PATTY (Beurskens et al., 1987) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTON (Spek, 1993), PLATON (Spek, 1990, 1995) ; _computing_publication_material ? _publ_section_experimental ; Crystal colour: red-brown transparant, crystal shape: irregular fragment. Profile analysis combining the methods of Lehman & Larsen (1974) and Grant & Gabe (1978). Empirical absorption correction using EMPABS (North, Phillips & Mathews, 1968). Data collection parameters: \w/2\q-scan with variable scan width, variable scan speed and variable aperture. Scan width (0.48 + 0.61tan\q)\%, range: 0.76\%-1.19\%, aperture (1.30 + 0.80tan\q)mm., range: 1.34-1.71mm. Maximum scan time: 30 sec/reflection. Least-squares refinement using calculated weights: w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+0.2109P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+0.2109P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.15(10) _refine_ls_number_reflns 2635 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0536 _refine_ls_R_factor_obs 0.0536 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_all 0.1609 _refine_ls_wR_factor_gt 0.1489 _refine_ls_wR_factor_obs 0.1489 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_shift/esd_mean 0.000 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 Rh1 Rh 0.92391(7) 0.90916(5) 0.94626(3) 0.0287(2) Uani 1 d . . . N1 N 1.0260(8) 1.0429(7) 0.9974(4) 0.0335(16) Uani 1 d . . . C2 C 0.9620(11) 1.1131(7) 1.0547(5) 0.042(2) Uani 1 d . . . H2 H 0.8594 1.1352 1.0434 0.051 Uiso 1 calc R . . C3 C 1.0657(14) 1.2171(9) 1.0521(7) 0.059(3) Uani 1 d . . . H3A H 1.0215 1.2774 1.0246 0.070 Uiso 1 calc R . . H3B H 1.0854 1.2453 1.0989 0.070 Uiso 1 calc R . . O4 O 1.2012(8) 1.1768(6) 1.0199(4) 0.0467(17) Uani 1 d . . . C5 C 1.1636(10) 1.0789(8) 0.9850(5) 0.0356(19) Uani 1 d . . . C6 C 1.2744(11) 1.0295(8) 0.9460(5) 0.044(2) Uani 1 d . . . H6 H 1.3671 1.0644 0.9438 0.053 Uiso 1 calc R . . C7 C 1.2525(10) 0.9301(7) 0.9102(5) 0.037(2) Uani 1 d . . . O8 O 1.3751(8) 0.8869(6) 0.8778(4) 0.0462(17) Uani 1 d . . . C9 C 1.3303(12) 0.7776(10) 0.8507(7) 0.053(3) Uani 1 d . . . H9A H 1.3620 0.7170 0.8816 0.064 Uiso 1 calc R . . H9B H 1.3721 0.7647 0.8046 0.064 Uiso 1 calc R . . C10 C 1.1625(10) 0.7846(8) 0.8475(5) 0.040(2) Uani 1 d . . . H10 H 1.1195 0.7119 0.8619 0.048 Uiso 1 calc R . . N11 N 1.1252(8) 0.8726(6) 0.9000(3) 0.0314(16) Uani 1 d . . . C11 C 0.9675(11) 1.0521(9) 1.1240(5) 0.045(2) Uani 1 d . . . C12 C 1.0792(13) 0.9746(9) 1.1413(5) 0.050(2) Uani 1 d . . . H12 H 1.1511 0.9556 1.1083 0.060 Uiso 1 calc R . . C13 C 1.0842(15) 0.9258(10) 1.2074(5) 0.058(3) Uani 1 d . . . H13 H 1.1573 0.8723 1.2175 0.069 Uiso 1 calc R . . C14 C 0.9864(19) 0.9540(12) 1.2564(6) 0.071(4) Uani 1 d . . . H14 H 0.9951 0.9241 1.3012 0.085 Uiso 1 calc R . . C15 C 0.8693(19) 1.0294(14) 1.2405(6) 0.082(5) Uani 1 d . . . H15 H 0.7968 1.0455 1.2738 0.099 Uiso 1 calc R . . C16 C 0.8627(13) 1.0789(12) 1.1754(6) 0.061(3) Uani 1 d . . . H16 H 0.7876 1.1308 1.1656 0.073 Uiso 1 calc R . . C21 C 1.1084(10) 0.8144(9) 0.7740(5) 0.042(2) Uani 1 d . . . C22 C 1.0870(14) 0.9230(11) 0.7528(5) 0.057(3) Uani 1 d . . . H22 H 1.0994 0.9814 0.7850 0.068 Uiso 1 calc R . . C23 C 1.0469(16) 0.9495(15) 0.6844(7) 0.076(4) Uani 1 d . . . H23 H 1.0284 1.0241 0.6713 0.092 Uiso 1 calc R . . C24 C 1.0354(17) 0.8636(19) 0.6373(6) 0.086(5) Uani 1 d . . . H24 H 1.0140 0.8804 0.5909 0.103 Uiso 1 calc R . . C25 C 1.0545(17) 0.7533(17) 0.6567(7) 0.087(5) Uani 1 d . . . H25 H 1.0412 0.6953 0.6244 0.104 Uiso 1 calc R . . C26 C 1.0940(15) 0.7284(12) 0.7253(7) 0.070(3) Uani 1 d . . . H26 H 1.1109 0.6536 0.7384 0.084 Uiso 1 calc R . . C31 C 0.8622(13) 0.7354(8) 0.9392(5) 0.049(2) Uani 1 d . . . H31A H 0.9424 0.6817 0.9313 0.059 Uiso 1 calc R . . H31B H 0.7883 0.7090 0.9724 0.059 Uiso 1 calc R . . C32 C 0.8084(10) 0.7923(8) 0.8803(5) 0.039(2) Uani 1 d . . . H32A H 0.7012 0.8014 0.8771 0.046 Uiso 1 calc R . . H32B H 0.8554 0.7741 0.8360 0.046 Uiso 1 calc R . . C33 C 0.7278(11) 0.9325(9) 1.0052(5) 0.048(2) Uani 1 d . . . H33A H 0.6576 0.8699 1.0054 0.057 Uiso 1 calc R . . H33B H 0.7395 0.9681 1.0506 0.057 Uiso 1 calc R . . C34 C 0.7217(10) 1.0047(10) 0.9479(6) 0.049(2) Uani 1 d . . . H34A H 0.7307 1.0852 0.9574 0.058 Uiso 1 calc R . . H34B H 0.6487 0.9869 0.9121 0.058 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0233(3) 0.0326(3) 0.0302(3) 0.0011(3) -0.0012(3) -0.0025(3) N1 0.026(3) 0.036(4) 0.039(4) -0.006(3) 0.000(3) -0.002(3) C2 0.040(5) 0.041(5) 0.046(5) -0.019(4) 0.002(4) -0.002(3) C3 0.070(7) 0.038(5) 0.068(6) -0.010(5) -0.003(8) 0.000(5) O4 0.044(4) 0.036(3) 0.061(4) -0.012(3) -0.004(4) -0.008(3) C5 0.039(5) 0.031(4) 0.037(4) 0.002(4) 0.000(4) -0.005(4) C6 0.030(4) 0.053(5) 0.049(5) 0.001(5) 0.002(5) -0.010(4) C7 0.038(5) 0.038(5) 0.035(4) 0.006(4) 0.005(4) 0.005(4) O8 0.031(3) 0.060(5) 0.047(4) -0.001(3) 0.012(3) 0.003(3) C9 0.040(6) 0.059(6) 0.061(7) -0.011(6) 0.002(5) 0.018(5) C10 0.039(5) 0.037(4) 0.044(5) -0.005(4) 0.008(4) 0.004(4) N11 0.029(4) 0.038(4) 0.027(3) 0.000(3) 0.002(3) -0.007(3) C11 0.041(6) 0.052(5) 0.042(5) -0.019(4) 0.009(4) -0.006(4) C12 0.045(6) 0.056(6) 0.048(5) -0.006(4) 0.008(5) 0.002(6) C13 0.062(7) 0.065(7) 0.045(5) 0.001(5) -0.005(5) 0.003(7) C14 0.102(11) 0.075(8) 0.036(5) -0.015(6) 0.004(6) 0.004(8) C15 0.098(11) 0.108(11) 0.041(6) -0.023(7) 0.029(7) -0.016(10) C16 0.043(6) 0.082(8) 0.056(6) -0.023(7) 0.012(5) 0.003(6) C21 0.025(5) 0.064(6) 0.037(4) -0.008(4) 0.006(4) -0.001(4) C22 0.060(7) 0.069(7) 0.041(5) 0.005(5) -0.002(5) -0.011(7) C23 0.075(10) 0.102(10) 0.053(7) 0.017(7) -0.009(7) 0.000(8) C24 0.065(9) 0.160(17) 0.034(6) -0.001(8) -0.004(6) 0.008(10) C25 0.089(11) 0.123(13) 0.049(6) -0.040(8) -0.006(7) 0.006(11) C26 0.064(8) 0.078(8) 0.069(7) -0.024(7) -0.001(7) 0.002(7) C31 0.064(6) 0.037(5) 0.046(5) -0.003(4) 0.009(5) -0.019(5) C32 0.024(4) 0.050(5) 0.042(5) -0.002(4) 0.000(4) -0.009(4) C33 0.028(4) 0.069(7) 0.046(5) -0.011(5) 0.004(4) -0.015(5) C34 0.020(4) 0.068(6) 0.058(6) -0.009(6) -0.010(5) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N11 2.056(7) . Y Rh1 N1 2.070(8) . Y Rh1 C33 2.108(10) . Y Rh1 C31 2.127(9) . Y Rh1 C34 2.136(9) . Y Rh1 C32 2.137(9) . Y N1 C5 1.326(11) . Y N1 C2 1.488(11) . Y C2 C11 1.510(15) . Y C2 C3 1.541(14) . Y C3 O4 1.443(13) . Y O4 C5 1.376(11) . Y C5 C6 1.372(13) . Y C6 C7 1.372(13) . Y C7 N11 1.342(12) . Y C7 O8 1.362(11) . Y O8 C9 1.446(14) . Y C9 C10 1.509(14) . Y C10 N11 1.483(11) . Y C10 C21 1.527(14) . Y C11 C16 1.396(14) . Y C11 C12 1.396(16) . Y C12 C13 1.390(14) . Y C13 C14 1.325(18) . Y C14 C15 1.41(2) . Y C15 C16 1.375(19) . Y C21 C22 1.358(15) . Y C21 C26 1.383(15) . Y C22 C23 1.391(15) . Y C23 C24 1.36(2) . Y C24 C25 1.36(2) . Y C25 C26 1.39(2) . Y C31 C32 1.396(15) . Y C33 C34 1.390(15) . Y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Rh1 N1 88.5(3) . . Y N11 Rh1 C33 172.1(4) . . Y N1 Rh1 C33 91.0(3) . . Y N11 Rh1 C31 90.0(4) . . Y N1 Rh1 C31 151.6(4) . . Y C33 Rh1 C31 86.7(4) . . Y N11 Rh1 C34 149.6(4) . . Y N1 Rh1 C34 88.1(4) . . Y C33 Rh1 C34 38.2(4) . . Y C31 Rh1 C34 106.8(5) . . Y N11 Rh1 C32 92.1(3) . . Y N1 Rh1 C32 170.1(3) . . Y C33 Rh1 C32 89.7(4) . . Y C31 Rh1 C32 38.2(4) . . Y C34 Rh1 C32 86.4(4) . . Y C5 N1 C2 108.2(7) . . Y C5 N1 Rh1 124.9(6) . . Y C2 N1 Rh1 126.9(6) . . Y N1 C2 C11 111.6(8) . . Y N1 C2 C3 100.8(8) . . Y C11 C2 C3 112.8(8) . . Y O4 C3 C2 105.1(7) . . Y C5 O4 C3 106.1(7) . . Y N1 C5 C6 129.4(9) . . Y N1 C5 O4 114.2(8) . . Y C6 C5 O4 116.3(8) . . Y C5 C6 C7 122.1(9) . . Y N11 C7 O8 115.7(8) . . Y N11 C7 C6 128.7(9) . . Y O8 C7 C6 115.6(9) . . Y C7 O8 C9 105.8(7) . . Y O8 C9 C10 104.1(8) . . Y N11 C10 C9 103.6(8) . . Y N11 C10 C21 112.9(8) . . Y C9 C10 C21 111.5(9) . . Y C7 N11 C10 105.0(7) . . Y C7 N11 Rh1 125.4(6) . . Y C10 N11 Rh1 129.5(6) . . Y C16 C11 C12 117.7(11) . . Y C16 C11 C2 119.2(10) . . Y C12 C11 C2 122.9(9) . . Y C13 C12 C11 120.6(10) . . Y C14 C13 C12 121.1(12) . . Y C13 C14 C15 120.0(12) . . Y C16 C15 C14 119.6(12) . . Y C15 C16 C11 120.7(13) . . Y C22 C21 C26 118.6(10) . . Y C22 C21 C10 122.4(9) . . Y C26 C21 C10 118.7(10) . . Y C21 C22 C23 121.9(12) . . Y C24 C23 C22 118.3(15) . . Y C23 C24 C25 121.4(12) . . Y C24 C25 C26 119.4(13) . . Y C21 C26 C25 120.2(14) . . Y C32 C31 Rh1 71.3(5) . . Y C31 C32 Rh1 70.5(5) . . Y C34 C33 Rh1 72.0(5) . . Y C33 C34 Rh1 69.8(6) . . Y _diffrn_reflns_theta_full 27.48 _refine_diff_density_max 1.828 _refine_diff_density_min -1.311 _refine_diff_density_rms 0.147 #===END