Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yasushi Tsuji' _publ_contact_author_address ; Department of Energy and Hydrocarbon Chemistry, Graduate School of Engineering Kyoto University Nishikyo-Ku Kyoto 615-8510 JAPAN ; _publ_contact_author_email YTSUJI@SCL.KYOTO-U.AC.JP _publ_section_title ; Rhodium(III) complexes with a bidentate N-heterocyclic carbene ligand bearing flexible dendritic frameworks ; loop_ _publ_author_name 'Yasushi Tsuji' 'Tetsuaki Fujihara' 'Yasushi Obora' 'Makoto Tokunaga' #============================================================================== data_3a _database_code_depnum_ccdc_archive 'CCDC 633257' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H31 I2 N4 O3 Rh ' _chemical_formula_moiety 'C23 H23 I2 N4 O2 Rh, C4 H8 O ' _chemical_formula_weight 816.28 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.126(5) _cell_length_b 14.786(6) _cell_length_c 15.987(6) _cell_angle_alpha 90.0000 _cell_angle_beta 92.446(6) _cell_angle_gamma 90.0000 _cell_volume 2863.8(20) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10056 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584.00 _exptl_absorpt_coefficient_mu 2.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.445 _exptl_absorpt_correction_T_max 0.573 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 20690 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 6455 _reflns_number_gt 5511 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0976 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6455 _refine_ls_number_parameters 365 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.29 _refine_diff_density_min -1.08 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; N N 0.006 0.003 ; 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) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.71961(3) 0.78271(2) 0.31406(2) 0.01800(8) Uani 1.00 1 d . . . I(2) I 0.46048(3) 0.49979(2) 0.24790(2) 0.01707(8) Uani 1.00 1 d . . . Rh(1) Rh 0.58600(3) 0.64173(3) 0.28606(2) 0.01257(9) Uani 1.00 1 d . . . O(1) O 0.6976(2) 0.5540(2) 0.3594(2) 0.0183(8) Uani 1.00 1 d . . . O(2) O 0.5639(2) 0.6235(2) 0.4213(2) 0.0183(8) Uani 1.00 1 d . . . O(3) O 0.9811(4) 0.1293(3) 0.0002(3) 0.0566(16) Uani 1.00 1 d . . . N(1) N 0.3642(3) 0.7299(2) 0.2796(2) 0.0160(10) Uani 1.00 1 d . . . N(2) N 0.4574(3) 0.7696(2) 0.1743(2) 0.0174(10) Uani 1.00 1 d . . . N(3) N 0.7036(3) 0.5821(2) 0.1348(2) 0.0158(10) Uani 1.00 1 d . . . N(4) N 0.6112(3) 0.7037(2) 0.1103(2) 0.0155(10) Uani 1.00 1 d . . . C(1) C 0.4634(3) 0.7190(3) 0.2453(2) 0.0142(11) Uani 1.00 1 d . . . C(2) C 0.2980(4) 0.7877(3) 0.2316(3) 0.0210(13) Uani 1.00 1 d . . . C(3) C 0.3566(4) 0.8127(3) 0.1656(3) 0.0199(12) Uani 1.00 1 d . . . C(4) C 0.6361(3) 0.6414(3) 0.1712(3) 0.0175(12) Uani 1.00 1 d . . . C(5) C 0.7222(4) 0.6079(3) 0.0525(3) 0.0192(12) Uani 1.00 1 d . . . C(6) C 0.6648(4) 0.6838(3) 0.0374(3) 0.0192(12) Uani 1.00 1 d . . . C(7) C 0.5501(4) 0.7859(3) 0.1224(2) 0.0171(12) Uani 1.00 1 d . . . C(8) C 0.3297(4) 0.6909(3) 0.3587(3) 0.0199(12) Uani 1.00 1 d . . . C(9) C 0.3183(4) 0.7630(3) 0.4244(3) 0.0178(12) Uani 1.00 1 d . . . C(10) C 0.4052(4) 0.8224(3) 0.4432(3) 0.0200(12) Uani 1.00 1 d . . . C(11) C 0.3959(4) 0.8867(3) 0.5059(3) 0.0227(13) Uani 1.00 1 d . . . C(12) C 0.2989(4) 0.8925(3) 0.5504(3) 0.0244(14) Uani 1.00 1 d . . . C(13) C 0.2131(4) 0.8332(3) 0.5316(3) 0.0275(15) Uani 1.00 1 d . . . C(14) C 0.2227(4) 0.7681(3) 0.4688(3) 0.0214(13) Uani 1.00 1 d . . . C(15) C 0.7565(4) 0.5021(3) 0.1739(3) 0.0195(12) Uani 1.00 1 d . . . C(16) C 0.8802(4) 0.5158(3) 0.1887(3) 0.0201(13) Uani 1.00 1 d . . . C(17) C 0.9203(4) 0.5735(3) 0.2514(3) 0.0287(15) Uani 1.00 1 d . . . C(18) C 1.0334(4) 0.5848(4) 0.2649(3) 0.0354(17) Uani 1.00 1 d . . . C(19) C 1.1065(4) 0.5381(4) 0.2166(3) 0.0374(17) Uani 1.00 1 d . . . C(20) C 1.0675(4) 0.4807(4) 0.1551(3) 0.0309(15) Uani 1.00 1 d . . . C(21) C 0.9540(4) 0.4690(3) 0.1403(3) 0.0250(14) Uani 1.00 1 d . . . C(22) C 0.6446(4) 0.5680(3) 0.4239(3) 0.0181(12) Uani 1.00 1 d . . . C(23) C 0.6736(4) 0.5186(3) 0.5042(3) 0.0262(14) Uani 1.00 1 d . . . C(24) C 0.9569(8) 0.0919(6) -0.0816(4) 0.076(3) Uani 1.00 1 d . . . C(25) C 0.9984(6) 0.1568(5) -0.1433(4) 0.056(2) Uani 1.00 1 d . . . C(26) C 1.0932(8) 0.1976(9) -0.0992(6) 0.114(4) Uani 1.00 1 d . . . C(27) C 1.0732(6) 0.1897(6) -0.0080(5) 0.072(2) Uani 1.00 1 d . . . H(1) H 0.2250 0.8060 0.2430 0.025 Uiso 1.00 1 c R . . H(2) H 0.3335 0.8528 0.1218 0.024 Uiso 1.00 1 c R . . H(3) H 0.7672 0.5768 0.0148 0.023 Uiso 1.00 1 c R . . H(4) H 0.6614 0.7175 -0.0132 0.023 Uiso 1.00 1 c R . . H(5) H 0.5974 0.8290 0.1497 0.021 Uiso 1.00 1 c R . . H(6) H 0.5245 0.8091 0.0697 0.020 Uiso 1.00 1 c R . . H(7) H 0.2608 0.6611 0.3495 0.024 Uiso 1.00 1 c R . . H(8) H 0.3838 0.6483 0.3778 0.024 Uiso 1.00 1 c R . . H(9) H 0.4702 0.8196 0.4122 0.024 Uiso 1.00 1 c R . . H(10) H 0.4559 0.9261 0.5195 0.027 Uiso 1.00 1 c R . . H(11) H 0.2919 0.9370 0.5927 0.029 Uiso 1.00 1 c R . . H(12) H 0.1473 0.8370 0.5616 0.033 Uiso 1.00 1 c R . . H(13) H 0.1638 0.7272 0.4568 0.026 Uiso 1.00 1 c R . . H(14) H 0.7249 0.4915 0.2264 0.023 Uiso 1.00 1 c R . . H(15) H 0.7443 0.4510 0.1387 0.023 Uiso 1.00 1 c R . . H(16) H 0.8704 0.6047 0.2854 0.035 Uiso 1.00 1 c R . . H(17) H 1.0606 0.6249 0.3074 0.042 Uiso 1.00 1 c R . . H(18) H 1.1838 0.5458 0.2262 0.045 Uiso 1.00 1 c R . . H(19) H 1.1179 0.4488 0.1221 0.037 Uiso 1.00 1 c R . . H(20) H 0.9271 0.4286 0.0981 0.030 Uiso 1.00 1 c R . . H(21) H 0.6325 0.4640 0.5062 0.032 Uiso 1.00 1 c R . . H(22) H 0.6560 0.5560 0.5501 0.032 Uiso 1.00 1 c R . . H(23) H 0.7503 0.5052 0.5073 0.032 Uiso 1.00 1 c R . . H(24) H 0.9933 0.0355 -0.0873 0.091 Uiso 1.00 1 c R . . H(25) H 0.8795 0.0836 -0.0897 0.091 Uiso 1.00 1 c R . . H(26) H 1.0169 0.1284 -0.1941 0.067 Uiso 1.00 1 c R . . H(27) H 0.9447 0.2024 -0.1548 0.067 Uiso 1.00 1 c R . . H(28) H 1.1567 0.1633 -0.1117 0.136 Uiso 1.00 1 c R . . H(29) H 1.1033 0.2586 -0.1160 0.136 Uiso 1.00 1 c R . . H(30) H 1.0554 0.2478 0.0131 0.085 Uiso 1.00 1 c R . . H(31) H 1.1363 0.1667 0.0222 0.085 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.02004(17) 0.01918(18) 0.01478(16) -0.00387(13) 0.00076(12) -0.00155(13) I(2) 0.01770(17) 0.01407(17) 0.01933(17) -0.00142(12) -0.00046(12) 0.00165(12) Rh(1) 0.01444(18) 0.01262(19) 0.01068(18) 0.00012(14) 0.00078(14) 0.00110(14) O(1) 0.0189(17) 0.0205(18) 0.0151(17) 0.0048(14) -0.0015(13) 0.0015(14) O(2) 0.0177(17) 0.0239(19) 0.0134(16) 0.0034(14) 0.0014(13) 0.0031(14) O(3) 0.063(3) 0.061(3) 0.045(3) 0.018(2) 0.006(2) -0.003(2) N(1) 0.018(2) 0.014(2) 0.016(2) 0.0020(16) 0.0002(16) 0.0002(16) N(2) 0.022(2) 0.014(2) 0.017(2) 0.0002(16) -0.0014(16) 0.0054(16) N(3) 0.018(2) 0.013(2) 0.017(2) 0.0005(16) 0.0005(16) 0.0000(16) N(4) 0.022(2) 0.014(2) 0.0111(19) 0.0005(16) 0.0020(16) 0.0012(16) C(1) 0.016(2) 0.012(2) 0.015(2) -0.0046(18) -0.0018(18) -0.0055(18) C(2) 0.016(2) 0.021(2) 0.026(2) 0.003(2) -0.004(2) 0.002(2) C(3) 0.019(2) 0.015(2) 0.025(2) 0.0008(19) -0.010(2) -0.001(2) C(4) 0.014(2) 0.021(2) 0.017(2) -0.0010(19) -0.0028(18) 0.001(2) C(5) 0.018(2) 0.026(2) 0.014(2) -0.004(2) 0.0058(19) -0.002(2) C(6) 0.024(2) 0.024(2) 0.010(2) -0.005(2) 0.0024(19) 0.001(2) C(7) 0.022(2) 0.018(2) 0.012(2) 0.002(2) 0.0016(19) 0.0041(19) C(8) 0.016(2) 0.022(2) 0.022(2) -0.003(2) -0.0002(19) 0.006(2) C(9) 0.020(2) 0.017(2) 0.017(2) 0.0041(19) -0.0001(19) 0.004(2) C(10) 0.016(2) 0.026(2) 0.018(2) -0.001(2) -0.0024(19) 0.005(2) C(11) 0.021(2) 0.023(2) 0.023(2) 0.002(2) -0.006(2) 0.001(2) C(12) 0.030(2) 0.024(2) 0.019(2) 0.006(2) 0.000(2) -0.000(2) C(13) 0.024(2) 0.037(3) 0.022(2) 0.004(2) 0.006(2) 0.000(2) C(14) 0.020(2) 0.027(2) 0.018(2) -0.001(2) 0.002(2) 0.006(2) C(15) 0.020(2) 0.019(2) 0.020(2) 0.005(2) -0.000(2) 0.002(2) C(16) 0.014(2) 0.025(2) 0.021(2) 0.004(2) 0.0021(19) 0.000(2) C(17) 0.021(2) 0.030(3) 0.035(3) -0.000(2) 0.005(2) -0.013(2) C(18) 0.022(2) 0.048(3) 0.035(3) -0.008(2) -0.003(2) -0.007(2) C(19) 0.018(2) 0.057(4) 0.037(3) 0.001(2) 0.004(2) 0.004(3) C(20) 0.025(2) 0.037(3) 0.031(3) 0.009(2) 0.007(2) -0.001(2) C(21) 0.024(2) 0.030(3) 0.021(2) 0.006(2) 0.003(2) 0.001(2) C(22) 0.018(2) 0.019(2) 0.017(2) -0.003(2) 0.0001(19) 0.002(2) C(23) 0.037(3) 0.026(2) 0.015(2) 0.011(2) 0.004(2) 0.006(2) C(24) 0.102(7) 0.082(6) 0.044(4) -0.044(5) 0.003(4) -0.009(4) C(25) 0.051(4) 0.067(5) 0.050(4) -0.011(3) 0.002(3) -0.010(4) C(26) 0.093(8) 0.188(12) 0.059(6) -0.088(8) -0.007(5) -0.003(7) C(27) 0.039(4) 0.107(7) 0.068(5) 0.002(4) -0.014(4) -0.036(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Rh(1) 2.6662(5) yes . . I(2) Rh(1) 2.6485(5) yes . . Rh(1) O(1) 2.181(3) yes . . Rh(1) O(2) 2.206(3) yes . . Rh(1) C(1) 1.964(4) yes . . Rh(1) C(4) 1.959(4) yes . . O(1) C(22) 1.254(5) yes . . O(2) C(22) 1.276(5) yes . . O(3) C(24) 1.438(9) yes . . O(3) C(27) 1.440(10) yes . . N(1) C(1) 1.353(6) yes . . N(1) C(2) 1.382(6) yes . . N(1) C(8) 1.467(6) yes . . N(2) C(1) 1.359(6) yes . . N(2) C(3) 1.381(6) yes . . N(2) C(7) 1.446(6) yes . . N(3) C(4) 1.348(6) yes . . N(3) C(5) 1.396(6) yes . . N(3) C(15) 1.473(6) yes . . N(4) C(4) 1.365(6) yes . . N(4) C(6) 1.389(6) yes . . N(4) C(7) 1.441(6) yes . . C(2) C(3) 1.349(7) yes . . C(5) C(6) 1.336(7) yes . . C(8) C(9) 1.507(7) yes . . C(9) C(10) 1.395(7) yes . . C(9) C(14) 1.387(7) yes . . C(10) C(11) 1.389(7) yes . . C(11) C(12) 1.403(7) yes . . C(12) C(13) 1.384(7) yes . . C(13) C(14) 1.399(7) yes . . C(15) C(16) 1.522(6) yes . . C(16) C(17) 1.389(7) yes . . C(16) C(21) 1.391(7) yes . . C(17) C(18) 1.390(7) yes . . C(18) C(19) 1.385(8) yes . . C(19) C(20) 1.368(8) yes . . C(20) C(21) 1.397(7) yes . . C(22) C(23) 1.506(7) yes . . C(24) C(25) 1.479(12) yes . . C(25) C(26) 1.454(13) yes . . C(26) C(27) 1.493(13) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(5) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(8) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(10) H(9) 0.950 no . . C(11) H(10) 0.950 no . . C(12) H(11) 0.950 no . . C(13) H(12) 0.950 no . . C(14) H(13) 0.950 no . . C(15) H(14) 0.950 no . . C(15) H(15) 0.950 no . . C(17) H(16) 0.950 no . . C(18) H(17) 0.950 no . . C(19) H(18) 0.950 no . . C(20) H(19) 0.950 no . . C(21) H(20) 0.950 no . . C(23) H(21) 0.950 no . . C(23) H(22) 0.950 no . . C(23) H(23) 0.950 no . . C(24) H(24) 0.950 no . . C(24) H(25) 0.950 no . . C(25) H(26) 0.950 no . . C(25) H(27) 0.950 no . . C(26) H(28) 0.950 no . . C(26) H(29) 0.950 no . . C(27) H(30) 0.950 no . . C(27) H(31) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I(1) Rh(1) I(2) 175.838(17) yes . . . I(1) Rh(1) O(1) 90.94(8) yes . . . I(1) Rh(1) O(2) 91.69(8) yes . . . I(1) Rh(1) C(1) 92.67(13) yes . . . I(1) Rh(1) C(4) 87.07(14) yes . . . I(2) Rh(1) O(1) 89.40(8) yes . . . I(2) Rh(1) O(2) 92.07(8) yes . . . I(2) Rh(1) C(1) 88.01(13) yes . . . I(2) Rh(1) C(4) 88.86(14) yes . . . O(1) Rh(1) O(2) 59.91(12) yes . . . O(1) Rh(1) C(1) 165.52(16) yes . . . O(1) Rh(1) C(4) 107.00(16) yes . . . O(2) Rh(1) C(1) 105.95(16) yes . . . O(2) Rh(1) C(4) 166.85(16) yes . . . C(1) Rh(1) C(4) 87.19(19) yes . . . Rh(1) O(1) C(22) 90.9(2) yes . . . Rh(1) O(2) C(22) 89.1(2) yes . . . C(24) O(3) C(27) 106.6(6) yes . . . C(1) N(1) C(2) 110.7(4) yes . . . C(1) N(1) C(8) 126.5(3) yes . . . C(2) N(1) C(8) 122.8(4) yes . . . C(1) N(2) C(3) 110.7(4) yes . . . C(1) N(2) C(7) 123.8(3) yes . . . C(3) N(2) C(7) 124.9(4) yes . . . C(4) N(3) C(5) 110.7(3) yes . . . C(4) N(3) C(15) 126.9(4) yes . . . C(5) N(3) C(15) 122.4(4) yes . . . C(4) N(4) C(6) 111.0(3) yes . . . C(4) N(4) C(7) 125.0(3) yes . . . C(6) N(4) C(7) 123.5(3) yes . . . Rh(1) C(1) N(1) 127.4(3) yes . . . Rh(1) C(1) N(2) 127.6(3) yes . . . N(1) C(1) N(2) 104.9(3) yes . . . N(1) C(2) C(3) 106.9(4) yes . . . N(2) C(3) C(2) 106.7(4) yes . . . Rh(1) C(4) N(3) 128.7(3) yes . . . Rh(1) C(4) N(4) 126.8(3) yes . . . N(3) C(4) N(4) 104.5(3) yes . . . N(3) C(5) C(6) 107.2(4) yes . . . N(4) C(6) C(5) 106.5(4) yes . . . N(2) C(7) N(4) 110.7(3) yes . . . N(1) C(8) C(9) 111.1(4) yes . . . C(8) C(9) C(10) 120.4(4) yes . . . C(8) C(9) C(14) 119.9(4) yes . . . C(10) C(9) C(14) 119.6(4) yes . . . C(9) C(10) C(11) 120.2(4) yes . . . C(10) C(11) C(12) 120.2(4) yes . . . C(11) C(12) C(13) 119.3(4) yes . . . C(12) C(13) C(14) 120.4(5) yes . . . C(9) C(14) C(13) 120.1(4) yes . . . N(3) C(15) C(16) 111.6(4) yes . . . C(15) C(16) C(17) 120.3(4) yes . . . C(15) C(16) C(21) 120.1(4) yes . . . C(17) C(16) C(21) 119.5(4) yes . . . C(16) C(17) C(18) 119.9(5) yes . . . C(17) C(18) C(19) 120.3(5) yes . . . C(18) C(19) C(20) 120.0(5) yes . . . C(19) C(20) C(21) 120.4(5) yes . . . C(16) C(21) C(20) 119.8(5) yes . . . O(1) C(22) O(2) 119.9(4) yes . . . O(1) C(22) C(23) 120.7(4) yes . . . O(2) C(22) C(23) 119.3(4) yes . . . O(3) C(24) C(25) 107.1(7) yes . . . C(24) C(25) C(26) 103.3(7) yes . . . C(25) C(26) C(27) 106.4(8) yes . . . O(3) C(27) C(26) 107.2(7) yes . . . N(1) C(2) H(1) 126.5 no . . . C(3) C(2) H(1) 126.6 no . . . N(2) C(3) H(2) 126.4 no . . . C(2) C(3) H(2) 126.8 no . . . N(3) C(5) H(3) 125.9 no . . . C(6) C(5) H(3) 126.9 no . . . N(4) C(6) H(4) 126.8 no . . . C(5) C(6) H(4) 126.7 no . . . N(2) C(7) H(5) 108.5 no . . . N(2) C(7) H(6) 109.6 no . . . N(4) C(7) H(5) 108.9 no . . . N(4) C(7) H(6) 109.7 no . . . H(5) C(7) H(6) 109.5 no . . . N(1) C(8) H(7) 109.3 no . . . N(1) C(8) H(8) 108.7 no . . . C(9) C(8) H(7) 109.2 no . . . C(9) C(8) H(8) 109.1 no . . . H(7) C(8) H(8) 109.5 no . . . C(9) C(10) H(9) 119.7 no . . . C(11) C(10) H(9) 120.0 no . . . C(10) C(11) H(10) 120.1 no . . . C(12) C(11) H(10) 119.7 no . . . C(11) C(12) H(11) 120.4 no . . . C(13) C(12) H(11) 120.3 no . . . C(12) C(13) H(12) 119.5 no . . . C(14) C(13) H(12) 120.0 no . . . C(9) C(14) H(13) 120.0 no . . . C(13) C(14) H(13) 119.9 no . . . N(3) C(15) H(14) 108.9 no . . . N(3) C(15) H(15) 109.5 no . . . C(16) C(15) H(14) 108.5 no . . . C(16) C(15) H(15) 108.9 no . . . H(14) C(15) H(15) 109.5 no . . . C(16) C(17) H(16) 120.0 no . . . C(18) C(17) H(16) 120.0 no . . . C(17) C(18) H(17) 119.7 no . . . C(19) C(18) H(17) 120.0 no . . . C(18) C(19) H(18) 120.0 no . . . C(20) C(19) H(18) 120.0 no . . . C(19) C(20) H(19) 119.7 no . . . C(21) C(20) H(19) 119.8 no . . . C(16) C(21) H(20) 119.9 no . . . C(20) C(21) H(20) 120.3 no . . . C(22) C(23) H(21) 109.7 no . . . C(22) C(23) H(22) 108.9 no . . . C(22) C(23) H(23) 109.8 no . . . H(21) C(23) H(22) 109.5 no . . . H(21) C(23) H(23) 109.5 no . . . H(22) C(23) H(23) 109.5 no . . . O(3) C(24) H(24) 110.3 no . . . O(3) C(24) H(25) 109.6 no . . . C(25) C(24) H(24) 109.5 no . . . C(25) C(24) H(25) 110.8 no . . . H(24) C(24) H(25) 109.5 no . . . C(24) C(25) H(26) 112.5 no . . . C(24) C(25) H(27) 109.9 no . . . C(26) C(25) H(26) 112.8 no . . . C(26) C(25) H(27) 108.7 no . . . H(26) C(25) H(27) 109.5 no . . . C(25) C(26) H(28) 107.9 no . . . C(25) C(26) H(29) 111.4 no . . . C(27) C(26) H(28) 109.3 no . . . C(27) C(26) H(29) 112.2 no . . . H(28) C(26) H(29) 109.5 no . . . O(3) C(27) H(30) 109.9 no . . . O(3) C(27) H(31) 110.0 no . . . C(26) C(27) H(30) 109.0 no . . . C(26) C(27) H(31) 111.2 no . . . H(30) C(27) H(31) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I(1) Rh(1) O(1) C(22) 93.5(2) ? . . . . I(1) Rh(1) O(2) C(22) -92.2(2) ? . . . . I(1) Rh(1) C(1) N(1) -116.5(3) ? . . . . I(1) Rh(1) C(1) N(2) 67.1(4) ? . . . . I(1) Rh(1) C(4) N(3) 107.7(4) ? . . . . I(1) Rh(1) C(4) N(4) -70.8(4) ? . . . . I(2) Rh(1) O(1) C(22) -90.6(2) ? . . . . I(2) Rh(1) O(2) C(22) 86.0(2) ? . . . . I(2) Rh(1) C(1) N(1) 67.6(4) ? . . . . I(2) Rh(1) C(1) N(2) -108.8(4) ? . . . . I(2) Rh(1) C(4) N(3) -71.4(4) ? . . . . I(2) Rh(1) C(4) N(4) 110.1(4) ? . . . . O(1) Rh(1) O(2) C(22) -2.1(2) ? . . . . O(2) Rh(1) O(1) C(22) 2.1(2) ? . . . . O(1) Rh(1) C(1) N(1) -12.3(9) ? . . . . O(1) Rh(1) C(1) N(2) 171.3(4) ? . . . . C(1) Rh(1) O(1) C(22) -11.0(7) ? . . . . O(1) Rh(1) C(4) N(3) 17.6(4) ? . . . . O(1) Rh(1) C(4) N(4) -160.9(3) ? . . . . C(4) Rh(1) O(1) C(22) -179.3(2) ? . . . . O(2) Rh(1) C(1) N(1) -24.0(4) ? . . . . O(2) Rh(1) C(1) N(2) 159.6(3) ? . . . . C(1) Rh(1) O(2) C(22) 174.5(2) ? . . . . O(2) Rh(1) C(4) N(3) 22.8(10) ? . . . . O(2) Rh(1) C(4) N(4) -155.7(5) ? . . . . C(4) Rh(1) O(2) C(22) -7.9(8) ? . . . . C(1) Rh(1) C(4) N(3) -159.5(4) ? . . . . C(1) Rh(1) C(4) N(4) 22.0(4) ? . . . . C(4) Rh(1) C(1) N(1) 156.5(4) ? . . . . C(4) Rh(1) C(1) N(2) -19.9(4) ? . . . . Rh(1) O(1) C(22) O(2) -3.7(4) ? . . . . Rh(1) O(1) C(22) C(23) 175.1(4) ? . . . . Rh(1) O(2) C(22) O(1) 3.6(4) ? . . . . Rh(1) O(2) C(22) C(23) -175.2(4) ? . . . . C(24) O(3) C(27) C(26) 7.9(9) ? . . . . C(27) O(3) C(24) C(25) -24.5(8) ? . . . . C(1) N(1) C(2) C(3) 0.5(5) ? . . . . C(2) N(1) C(1) Rh(1) -178.1(3) ? . . . . C(2) N(1) C(1) N(2) -1.0(5) ? . . . . C(1) N(1) C(8) C(9) 110.5(5) ? . . . . C(8) N(1) C(1) Rh(1) 4.6(6) ? . . . . C(8) N(1) C(1) N(2) -178.3(4) ? . . . . C(2) N(1) C(8) C(9) -66.5(5) ? . . . . C(8) N(1) C(2) C(3) 177.9(4) ? . . . . C(1) N(2) C(3) C(2) -0.8(5) ? . . . . C(3) N(2) C(1) Rh(1) 178.2(3) ? . . . . C(3) N(2) C(1) N(1) 1.1(5) ? . . . . C(1) N(2) C(7) N(4) 44.1(5) ? . . . . C(7) N(2) C(1) Rh(1) -10.2(6) ? . . . . C(7) N(2) C(1) N(1) 172.8(3) ? . . . . C(3) N(2) C(7) N(4) -145.5(4) ? . . . . C(7) N(2) C(3) C(2) -172.4(4) ? . . . . C(4) N(3) C(5) C(6) -0.5(5) ? . . . . C(5) N(3) C(4) Rh(1) -177.8(3) ? . . . . C(5) N(3) C(4) N(4) 1.0(5) ? . . . . C(4) N(3) C(15) C(16) -108.7(5) ? . . . . C(15) N(3) C(4) Rh(1) -0.0(6) ? . . . . C(15) N(3) C(4) N(4) 178.7(4) ? . . . . C(5) N(3) C(15) C(16) 68.7(5) ? . . . . C(15) N(3) C(5) C(6) -178.3(4) ? . . . . C(4) N(4) C(6) C(5) 0.9(5) ? . . . . C(6) N(4) C(4) Rh(1) 177.6(3) ? . . . . C(6) N(4) C(4) N(3) -1.2(5) ? . . . . C(4) N(4) C(7) N(2) -41.9(5) ? . . . . C(7) N(4) C(4) Rh(1) 5.6(6) ? . . . . C(7) N(4) C(4) N(3) -173.2(4) ? . . . . C(6) N(4) C(7) N(2) 147.0(4) ? . . . . C(7) N(4) C(6) C(5) 173.1(4) ? . . . . N(1) C(2) C(3) N(2) 0.2(4) ? . . . . N(3) C(5) C(6) N(4) -0.3(5) ? . . . . N(1) C(8) C(9) C(10) -53.0(5) ? . . . . N(1) C(8) C(9) C(14) 129.6(4) ? . . . . C(8) C(9) C(10) C(11) -177.6(4) ? . . . . C(8) C(9) C(14) C(13) 178.1(4) ? . . . . C(10) C(9) C(14) C(13) 0.6(7) ? . . . . C(14) C(9) C(10) C(11) -0.2(6) ? . . . . C(9) C(10) C(11) C(12) -0.5(7) ? . . . . C(10) C(11) C(12) C(13) 0.7(7) ? . . . . C(11) C(12) C(13) C(14) -0.2(6) ? . . . . C(12) C(13) C(14) C(9) -0.4(7) ? . . . . N(3) C(15) C(16) C(17) 72.6(6) ? . . . . N(3) C(15) C(16) C(21) -108.6(5) ? . . . . C(15) C(16) C(17) C(18) 179.3(5) ? . . . . C(15) C(16) C(21) C(20) -178.9(5) ? . . . . C(17) C(16) C(21) C(20) -0.2(6) ? . . . . C(21) C(16) C(17) C(18) 0.6(8) ? . . . . C(16) C(17) C(18) C(19) -0.6(9) ? . . . . C(17) C(18) C(19) C(20) 0.2(7) ? . . . . C(18) C(19) C(20) C(21) 0.3(7) ? . . . . C(19) C(20) C(21) C(16) -0.3(7) ? . . . . O(3) C(24) C(25) C(26) 31.3(9) ? . . . . C(24) C(25) C(26) C(27) -25.7(10) ? . . . . C(25) C(26) C(27) O(3) 11.7(10) ? . . . . #============================================================================== data_3b _database_code_depnum_ccdc_archive 'CCDC 633258' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C53 H50 I2 N5 O6 Rh ' _chemical_formula_moiety 'C51 H47 I2 N4 O6 Rh, C2 H3 N ' _chemical_formula_weight 1209.72 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.338(4) _cell_length_b 13.972(6) _cell_length_c 20.243(8) _cell_angle_alpha 72.083(12) _cell_angle_beta 85.573(14) _cell_angle_gamma 78.379(9) _cell_volume 2461.0(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7837 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204.00 _exptl_absorpt_coefficient_mu 1.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.718 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 16404 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.919 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 10345 _reflns_number_gt 8789 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1017 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10345 _refine_ls_number_parameters 654 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.13 _refine_diff_density_min -0.85 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; N N 0.006 0.003 ; 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) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.78396(3) -0.05952(2) 0.413830(10) 0.01673(7) Uani 1.00 1 d . . . I(2) I 0.55259(3) 0.30311(2) 0.245700(10) 0.01719(6) Uani 1.00 1 d . . . Rh(1) Rh 0.66070(3) 0.12100(2) 0.33164(2) 0.01116(7) Uani 1.00 1 d . . . O(1) O 0.8775(2) 0.1487(2) 0.29703(14) 0.0170(7) Uani 1.00 1 d . . . O(2) O 0.7598(2) 0.0745(2) 0.24351(14) 0.0157(7) Uani 1.00 1 d . . . O(3) O 1.1283(3) 0.3826(2) 0.51856(15) 0.0206(7) Uani 1.00 1 d . . . O(4) O 0.9929(3) 0.4789(2) 0.28146(15) 0.0236(8) Uani 1.00 1 d . . . O(5) O 0.1764(3) -0.1039(2) 0.13519(14) 0.0190(7) Uani 1.00 1 d . . . O(6) O 0.4544(3) 0.1612(2) 0.04784(14) 0.0205(7) Uani 1.00 1 d . . . N(1) N 0.7040(3) 0.1858(2) 0.45583(17) 0.0146(8) Uani 1.00 1 d . . . N(2) N 0.4769(3) 0.2000(2) 0.43801(16) 0.0140(8) Uani 1.00 1 d . . . N(3) N 0.4256(3) 0.0033(2) 0.32974(16) 0.0141(8) Uani 1.00 1 d . . . N(4) N 0.3504(3) 0.1193(2) 0.37939(17) 0.0155(8) Uani 1.00 1 d . . . N(5) N 0.1952(5) 0.7410(4) 0.3579(2) 0.0457(15) Uani 1.00 1 d . . . C(1) C 0.6116(4) 0.1727(2) 0.4123(2) 0.0134(9) Uani 1.00 1 d . . . C(2) C 0.6254(4) 0.2204(3) 0.5080(2) 0.0168(10) Uani 1.00 1 d . . . C(3) C 0.4830(4) 0.2295(3) 0.4969(2) 0.0189(10) Uani 1.00 1 d . . . C(4) C 0.4689(4) 0.0789(3) 0.34698(19) 0.0137(9) Uani 1.00 1 d . . . C(5) C 0.2804(4) -0.0018(3) 0.3503(2) 0.0179(10) Uani 1.00 1 d . . . C(6) C 0.2338(4) 0.0704(3) 0.3812(2) 0.0200(10) Uani 1.00 1 d . . . C(7) C 0.3427(4) 0.2075(3) 0.4030(2) 0.0175(10) Uani 1.00 1 d . . . C(8) C 0.8645(4) 0.1656(3) 0.4504(2) 0.0180(10) Uani 1.00 1 d . . . C(9) C 0.9275(4) 0.2617(3) 0.4317(2) 0.0151(9) Uani 1.00 1 d . . . C(10) C 0.9914(4) 0.2864(3) 0.4831(2) 0.0144(9) Uani 1.00 1 d . . . C(11) C 1.0619(4) 0.3696(3) 0.4643(2) 0.0147(9) Uani 1.00 1 d . . . C(12) C 1.0616(4) 0.4325(3) 0.3969(2) 0.0184(10) Uani 1.00 1 d . . . C(13) C 0.9914(4) 0.4099(3) 0.3466(2) 0.0178(10) Uani 1.00 1 d . . . C(14) C 0.9290(4) 0.3238(3) 0.3626(2) 0.0184(10) Uani 1.00 1 d . . . C(15) C 1.2258(4) 0.4541(3) 0.5020(2) 0.0182(10) Uani 1.00 1 d . . . C(16) C 1.3008(4) 0.4454(3) 0.5671(2) 0.0192(10) Uani 1.00 1 d . . . C(17) C 1.3027(4) 0.3624(3) 0.6267(2) 0.0248(11) Uani 1.00 1 d . . . C(18) C 1.3725(5) 0.3592(3) 0.6858(2) 0.0290(12) Uani 1.00 1 d . . . C(19) C 1.4394(5) 0.4392(3) 0.6861(2) 0.0291(13) Uani 1.00 1 d . . . C(20) C 1.4381(5) 0.5209(3) 0.6267(2) 0.0283(13) Uani 1.00 1 d . . . C(21) C 1.3702(4) 0.5239(3) 0.5678(2) 0.0213(11) Uani 1.00 1 d . . . C(22) C 0.9026(4) 0.4745(3) 0.2292(2) 0.0239(11) Uani 1.00 1 d . . . C(23) C 0.9826(4) 0.4166(3) 0.1814(2) 0.0194(10) Uani 1.00 1 d . . . C(24) C 0.9164(5) 0.4230(3) 0.1211(2) 0.0271(12) Uani 1.00 1 d . . . C(25) C 0.9876(5) 0.3735(3) 0.0748(2) 0.0303(13) Uani 1.00 1 d . . . C(26) C 1.1282(4) 0.3160(3) 0.0885(2) 0.0260(12) Uani 1.00 1 d . . . C(27) C 1.1933(4) 0.3090(3) 0.1492(2) 0.0233(11) Uani 1.00 1 d . . . C(28) C 1.1221(4) 0.3580(3) 0.1954(2) 0.0215(11) Uani 1.00 1 d . . . C(29) C 0.5111(4) -0.0621(3) 0.2902(2) 0.0171(10) Uani 1.00 1 d . . . C(30) C 0.4482(4) -0.0325(3) 0.2182(2) 0.0154(9) Uani 1.00 1 d . . . C(31) C 0.3481(4) -0.0844(3) 0.2051(2) 0.0167(10) Uani 1.00 1 d . . . C(32) C 0.2812(4) -0.0503(3) 0.1405(2) 0.0157(9) Uani 1.00 1 d . . . C(33) C 0.3198(4) 0.0306(3) 0.0884(2) 0.0159(10) Uani 1.00 1 d . . . C(34) C 0.4239(4) 0.0815(3) 0.1023(2) 0.0162(10) Uani 1.00 1 d . . . C(35) C 0.4865(4) 0.0516(3) 0.1668(2) 0.0157(9) Uani 1.00 1 d . . . C(36) C 0.0947(4) -0.0679(3) 0.0718(2) 0.0183(10) Uani 1.00 1 d . . . C(37) C -0.0229(4) -0.1310(3) 0.0824(2) 0.0178(10) Uani 1.00 1 d . . . C(38) C -0.1597(4) -0.0982(3) 0.1075(2) 0.0205(10) Uani 1.00 1 d . . . C(39) C -0.2674(4) -0.1588(3) 0.1188(2) 0.0234(11) Uani 1.00 1 d . . . C(40) C -0.2354(4) -0.2523(3) 0.1059(2) 0.0226(11) Uani 1.00 1 d . . . C(41) C -0.0982(4) -0.2858(3) 0.0810(2) 0.0197(10) Uani 1.00 1 d . . . C(42) C 0.0077(4) -0.2246(3) 0.0685(2) 0.0183(10) Uani 1.00 1 d . . . C(43) C 0.5643(4) 0.2132(3) 0.0582(2) 0.0184(10) Uani 1.00 1 d . . . C(44) C 0.5932(4) 0.2897(3) -0.0100(2) 0.0189(10) Uani 1.00 1 d . . . C(45) C 0.6290(5) 0.3819(3) -0.0113(2) 0.0290(13) Uani 1.00 1 d . . . C(46) C 0.6642(5) 0.4497(3) -0.0742(2) 0.0357(14) Uani 1.00 1 d . . . C(47) C 0.6664(5) 0.4252(3) -0.1355(2) 0.0336(13) Uani 1.00 1 d . . . C(48) C 0.6312(4) 0.3333(3) -0.1344(2) 0.0290(12) Uani 1.00 1 d . . . C(49) C 0.5957(4) 0.2647(3) -0.0717(2) 0.0211(10) Uani 1.00 1 d . . . C(50) C 0.8740(4) 0.1073(3) 0.2495(2) 0.0169(10) Uani 1.00 1 d . . . C(51) C 1.0018(4) 0.0968(3) 0.2014(2) 0.0257(12) Uani 1.00 1 d . . . C(52) C 0.0140(6) 0.7323(5) 0.2708(2) 0.0538(19) Uani 1.00 1 d . . . C(53) C 0.1153(5) 0.7370(4) 0.3207(2) 0.0338(14) Uani 1.00 1 d . . . H(1) H 0.6655 0.2350 0.5448 0.021 Uiso 1.00 1 c R . . H(2) H 0.4027 0.2516 0.5239 0.024 Uiso 1.00 1 c R . . H(3) H 0.2255 -0.0484 0.3438 0.022 Uiso 1.00 1 c R . . H(4) H 0.1392 0.0857 0.4006 0.025 Uiso 1.00 1 c R . . H(5) H 0.2621 0.2114 0.4343 0.021 Uiso 1.00 1 c R . . H(6) H 0.3299 0.2675 0.3642 0.021 Uiso 1.00 1 c R . . H(7) H 0.9027 0.1218 0.4938 0.021 Uiso 1.00 1 c R . . H(8) H 0.8929 0.1325 0.4156 0.021 Uiso 1.00 1 c R . . H(9) H 0.9863 0.2467 0.5303 0.018 Uiso 1.00 1 c R . . H(10) H 1.1082 0.4902 0.3850 0.023 Uiso 1.00 1 c R . . H(11) H 0.8867 0.3069 0.3275 0.024 Uiso 1.00 1 c R . . H(12) H 1.2966 0.4388 0.4686 0.023 Uiso 1.00 1 c R . . H(13) H 1.1720 0.5216 0.4837 0.023 Uiso 1.00 1 c R . . H(14) H 1.2566 0.3075 0.6270 0.030 Uiso 1.00 1 c R . . H(15) H 1.3749 0.3017 0.7261 0.034 Uiso 1.00 1 c R . . H(16) H 1.4849 0.4378 0.7269 0.037 Uiso 1.00 1 c R . . H(17) H 1.4842 0.5757 0.6265 0.037 Uiso 1.00 1 c R . . H(18) H 1.3718 0.5803 0.5272 0.027 Uiso 1.00 1 c R . . H(19) H 0.8244 0.4417 0.2514 0.028 Uiso 1.00 1 c R . . H(20) H 0.8643 0.5425 0.2021 0.028 Uiso 1.00 1 c R . . H(21) H 0.8207 0.4622 0.1110 0.033 Uiso 1.00 1 c R . . H(22) H 0.9403 0.3786 0.0336 0.037 Uiso 1.00 1 c R . . H(23) H 1.1783 0.2826 0.0567 0.032 Uiso 1.00 1 c R . . H(24) H 1.2888 0.2695 0.1594 0.028 Uiso 1.00 1 c R . . H(25) H 1.1689 0.3515 0.2371 0.027 Uiso 1.00 1 c R . . H(26) H 0.6099 -0.0530 0.2863 0.021 Uiso 1.00 1 c R . . H(27) H 0.5072 -0.1318 0.3136 0.021 Uiso 1.00 1 c R . . H(28) H 0.3252 -0.1431 0.2397 0.020 Uiso 1.00 1 c R . . H(29) H 0.2767 0.0516 0.0440 0.020 Uiso 1.00 1 c R . . H(30) H 0.5546 0.0878 0.1761 0.019 Uiso 1.00 1 c R . . H(31) H 0.0526 0.0026 0.0627 0.021 Uiso 1.00 1 c R . . H(32) H 0.1571 -0.0774 0.0341 0.022 Uiso 1.00 1 c R . . H(33) H -0.1809 -0.0344 0.1172 0.024 Uiso 1.00 1 c R . . H(34) H -0.3618 -0.1356 0.1356 0.027 Uiso 1.00 1 c R . . H(35) H -0.3078 -0.2937 0.1139 0.028 Uiso 1.00 1 c R . . H(36) H -0.0760 -0.3504 0.0724 0.025 Uiso 1.00 1 c R . . H(37) H 0.1013 -0.2469 0.0507 0.022 Uiso 1.00 1 c R . . H(38) H 0.5313 0.2478 0.0918 0.023 Uiso 1.00 1 c R . . H(39) H 0.6516 0.1651 0.0737 0.023 Uiso 1.00 1 c R . . H(40) H 0.6299 0.3988 0.0306 0.036 Uiso 1.00 1 c R . . H(41) H 0.6864 0.5135 -0.0750 0.041 Uiso 1.00 1 c R . . H(42) H 0.6918 0.4713 -0.1781 0.036 Uiso 1.00 1 c R . . H(43) H 0.6311 0.3167 -0.1765 0.032 Uiso 1.00 1 c R . . H(44) H 0.5737 0.2011 -0.0713 0.024 Uiso 1.00 1 c R . . H(45) H 0.9924 0.1560 0.1621 0.033 Uiso 1.00 1 c R . . H(46) H 1.0055 0.0379 0.1868 0.033 Uiso 1.00 1 c R . . H(47) H 1.0891 0.0901 0.2250 0.033 Uiso 1.00 1 c R . . H(48) H -0.0451 0.7981 0.2528 0.066 Uiso 1.00 1 c R . . H(49) H -0.0465 0.6842 0.2931 0.066 Uiso 1.00 1 c R . . H(50) H 0.0679 0.7122 0.2340 0.066 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.01607(14) 0.01500(14) 0.01779(15) -0.00284(10) -0.00439(10) -0.00203(10) I(2) 0.01885(14) 0.01648(14) 0.01459(14) -0.00253(10) -0.00340(11) -0.00202(10) Rh(1) 0.00936(14) 0.01380(15) 0.01076(16) -0.0029(1) -0.0001(1) -0.0038(1) O(1) 0.0136(13) 0.0220(15) 0.0182(15) -0.0070(11) 0.0035(11) -0.0083(12) O(2) 0.0125(13) 0.0213(15) 0.0148(14) -0.0033(11) 0.0012(11) -0.0077(11) O(3) 0.0234(15) 0.0247(16) 0.0173(15) -0.0135(12) 0.0006(12) -0.0062(12) O(4) 0.0353(17) 0.0232(16) 0.0133(15) -0.0106(13) -0.0080(13) -0.0015(12) O(5) 0.0226(15) 0.0232(15) 0.0130(14) -0.0102(12) -0.0028(11) -0.0035(12) O(6) 0.0237(15) 0.0254(16) 0.0142(14) -0.0153(12) -0.0049(12) -0.0004(12) N(1) 0.0126(15) 0.0180(17) 0.0127(17) -0.0043(13) -0.0002(13) -0.0027(13) N(2) 0.0126(15) 0.0187(17) 0.0125(16) -0.0024(13) 0.0012(13) -0.0077(13) N(3) 0.0106(15) 0.0208(17) 0.0102(16) -0.0031(13) -0.0011(12) -0.0032(13) N(4) 0.0109(15) 0.0216(18) 0.0140(17) -0.0020(13) -0.0008(13) -0.0056(14) N(5) 0.046(2) 0.073(3) 0.028(2) -0.030(2) 0.006(2) -0.019(2) C(1) 0.0145(18) 0.0126(18) 0.0122(19) -0.0043(14) -0.0011(15) -0.0012(15) C(2) 0.022(2) 0.016(2) 0.014(2) -0.0079(16) 0.0031(16) -0.0041(16) C(3) 0.022(2) 0.020(2) 0.018(2) -0.0078(17) 0.0069(17) -0.0093(17) C(4) 0.0107(17) 0.019(2) 0.0092(18) 0.0018(15) -0.0039(14) -0.0024(15) C(5) 0.0122(18) 0.027(2) 0.016(2) -0.0079(16) 0.0007(16) -0.0061(17) C(6) 0.0105(18) 0.029(2) 0.023(2) -0.0089(17) 0.0011(16) -0.0086(18) C(7) 0.0129(18) 0.020(2) 0.020(2) -0.0011(16) 0.0006(16) -0.0068(17) C(8) 0.0117(18) 0.020(2) 0.022(2) -0.0019(15) -0.0039(16) -0.0043(17) C(9) 0.0092(17) 0.019(2) 0.019(2) -0.0015(15) 0.0017(15) -0.0086(16) C(10) 0.0137(18) 0.022(2) 0.0092(19) -0.0058(15) 0.0007(15) -0.0054(16) C(11) 0.0101(17) 0.020(2) 0.018(2) -0.0021(15) -0.0054(15) -0.0105(16) C(12) 0.022(2) 0.021(2) 0.014(2) -0.0066(17) -0.0004(16) -0.0059(17) C(13) 0.022(2) 0.018(2) 0.0103(19) 0.0007(16) 0.0003(16) -0.0028(16) C(14) 0.018(2) 0.023(2) 0.017(2) -0.0050(17) -0.0027(17) -0.0103(17) C(15) 0.020(2) 0.019(2) 0.018(2) -0.0069(16) -0.0019(17) -0.0068(17) C(16) 0.0151(19) 0.022(2) 0.022(2) -0.0017(16) -0.0017(17) -0.0100(18) C(17) 0.028(2) 0.024(2) 0.024(2) -0.0095(19) 0.0003(19) -0.0070(18) C(18) 0.034(2) 0.029(2) 0.023(2) -0.003(2) -0.007(2) -0.007(2) C(19) 0.025(2) 0.041(2) 0.027(2) -0.001(2) -0.007(2) -0.019(2) C(20) 0.028(2) 0.034(2) 0.031(2) -0.009(2) -0.001(2) -0.018(2) C(21) 0.021(2) 0.019(2) 0.026(2) -0.0080(17) -0.0018(18) -0.0074(18) C(22) 0.028(2) 0.026(2) 0.016(2) -0.0050(19) -0.0023(18) -0.0028(18) C(23) 0.023(2) 0.021(2) 0.015(2) -0.0104(17) 0.0013(17) -0.0031(17) C(24) 0.022(2) 0.035(2) 0.024(2) -0.0038(19) -0.0062(19) -0.008(2) C(25) 0.034(2) 0.039(2) 0.020(2) -0.004(2) -0.005(2) -0.014(2) C(26) 0.025(2) 0.033(2) 0.022(2) -0.004(2) 0.0024(19) -0.014(2) C(27) 0.021(2) 0.025(2) 0.025(2) -0.0040(18) 0.0010(18) -0.0095(19) C(28) 0.021(2) 0.028(2) 0.018(2) -0.0120(18) -0.0060(17) -0.0045(18) C(29) 0.0175(19) 0.017(2) 0.016(2) -0.0038(16) -0.0025(16) -0.0041(16) C(30) 0.0165(19) 0.020(2) 0.0112(19) -0.0036(16) -0.0010(15) -0.0072(16) C(31) 0.0171(19) 0.018(2) 0.014(2) -0.0047(16) 0.0031(16) -0.0032(16) C(32) 0.0148(19) 0.020(2) 0.015(2) -0.0053(16) 0.0009(15) -0.0082(16) C(33) 0.0149(19) 0.020(2) 0.015(2) -0.0046(16) 0.0000(15) -0.0076(16) C(34) 0.0150(19) 0.020(2) 0.014(2) -0.0074(16) 0.0019(15) -0.0039(16) C(35) 0.0143(18) 0.019(2) 0.014(2) -0.0070(15) 0.0016(15) -0.0040(16) C(36) 0.017(2) 0.025(2) 0.012(2) -0.0078(17) -0.0025(16) -0.0006(16) C(37) 0.019(2) 0.022(2) 0.0101(19) -0.0062(17) -0.0060(16) 0.0005(16) C(38) 0.018(2) 0.024(2) 0.019(2) -0.0057(17) 0.0001(17) -0.0046(17) C(39) 0.017(2) 0.028(2) 0.022(2) -0.0034(18) -0.0007(17) -0.0031(18) C(40) 0.021(2) 0.030(2) 0.019(2) -0.0138(18) -0.0003(17) -0.0065(18) C(41) 0.023(2) 0.022(2) 0.017(2) -0.0069(17) -0.0004(17) -0.0075(17) C(42) 0.0148(19) 0.027(2) 0.014(2) -0.0060(16) -0.0013(16) -0.0057(17) C(43) 0.017(2) 0.019(2) 0.021(2) -0.0105(16) 0.0004(16) -0.0034(17) C(44) 0.0132(19) 0.019(2) 0.023(2) -0.0054(16) -0.0034(16) -0.0019(17) C(45) 0.033(2) 0.025(2) 0.031(2) -0.011(2) 0.000(2) -0.009(2) C(46) 0.042(2) 0.021(2) 0.040(3) -0.013(2) 0.004(2) -0.001(2) C(47) 0.032(2) 0.029(2) 0.029(2) -0.008(2) -0.000(2) 0.009(2) C(48) 0.023(2) 0.036(2) 0.021(2) -0.003(2) -0.0040(18) 0.002(2) C(49) 0.018(2) 0.022(2) 0.019(2) -0.0026(17) -0.0036(17) -0.0002(17) C(50) 0.018(2) 0.018(2) 0.013(2) -0.0056(16) -0.0007(16) -0.0015(16) C(51) 0.019(2) 0.036(2) 0.027(2) -0.0127(19) 0.0081(18) -0.014(2) C(52) 0.061(3) 0.069(4) 0.034(3) -0.041(3) -0.005(2) -0.001(2) C(53) 0.042(2) 0.044(3) 0.024(2) -0.027(2) 0.012(2) -0.012(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Rh(1) 2.6454(3) yes . . I(2) Rh(1) 2.6518(3) yes . . Rh(1) O(1) 2.161(2) yes . . Rh(1) O(2) 2.163(2) yes . . Rh(1) C(1) 1.969(4) yes . . Rh(1) C(4) 1.969(4) yes . . O(1) C(50) 1.272(5) yes . . O(2) C(50) 1.269(5) yes . . O(3) C(11) 1.377(5) yes . . O(3) C(15) 1.432(5) yes . . O(4) C(13) 1.374(4) yes . . O(4) C(22) 1.426(6) yes . . O(5) C(32) 1.375(5) yes . . O(5) C(36) 1.442(4) yes . . O(6) C(34) 1.364(4) yes . . O(6) C(43) 1.432(5) yes . . N(1) C(1) 1.355(5) yes . . N(1) C(2) 1.393(5) yes . . N(1) C(8) 1.470(4) yes . . N(2) C(1) 1.351(4) yes . . N(2) C(3) 1.384(6) yes . . N(2) C(7) 1.457(5) yes . . N(3) C(4) 1.349(6) yes . . N(3) C(5) 1.397(5) yes . . N(3) C(29) 1.473(5) yes . . N(4) C(4) 1.356(4) yes . . N(4) C(6) 1.390(6) yes . . N(4) C(7) 1.439(6) yes . . N(5) C(53) 1.121(7) yes . . C(2) C(3) 1.340(6) yes . . C(5) C(6) 1.330(6) yes . . C(8) C(9) 1.505(6) yes . . C(9) C(10) 1.399(6) yes . . C(9) C(14) 1.401(5) yes . . C(10) C(11) 1.388(6) yes . . C(11) C(12) 1.377(5) yes . . C(12) C(13) 1.398(6) yes . . C(13) C(14) 1.381(6) yes . . C(15) C(16) 1.501(6) yes . . C(16) C(17) 1.392(5) yes . . C(16) C(21) 1.386(7) yes . . C(17) C(18) 1.391(7) yes . . C(18) C(19) 1.387(8) yes . . C(19) C(20) 1.379(6) yes . . C(20) C(21) 1.378(7) yes . . C(22) C(23) 1.509(6) yes . . C(23) C(24) 1.381(6) yes . . C(23) C(28) 1.390(5) yes . . C(24) C(25) 1.384(7) yes . . C(25) C(26) 1.393(6) yes . . C(26) C(27) 1.381(6) yes . . C(27) C(28) 1.379(6) yes . . C(29) C(30) 1.518(5) yes . . C(30) C(31) 1.379(6) yes . . C(30) C(35) 1.396(5) yes . . C(31) C(32) 1.397(5) yes . . C(32) C(33) 1.375(5) yes . . C(33) C(34) 1.406(6) yes . . C(34) C(35) 1.379(5) yes . . C(36) C(37) 1.506(6) yes . . C(37) C(38) 1.380(5) yes . . C(37) C(42) 1.390(6) yes . . C(38) C(39) 1.403(6) yes . . C(39) C(40) 1.381(7) yes . . C(40) C(41) 1.385(5) yes . . C(41) C(42) 1.394(6) yes . . C(43) C(44) 1.507(5) yes . . C(44) C(45) 1.388(7) yes . . C(44) C(49) 1.393(6) yes . . C(45) C(46) 1.395(6) yes . . C(46) C(47) 1.382(8) yes . . C(47) C(48) 1.381(8) yes . . C(48) C(49) 1.397(5) yes . . C(50) C(51) 1.494(5) yes . . C(52) C(53) 1.459(9) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(5) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(8) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(10) H(9) 0.950 no . . C(12) H(10) 0.950 no . . C(14) H(11) 0.950 no . . C(15) H(12) 0.950 no . . C(15) H(13) 0.950 no . . C(17) H(14) 0.950 no . . C(18) H(15) 0.950 no . . C(19) H(16) 0.950 no . . C(20) H(17) 0.950 no . . C(21) H(18) 0.950 no . . C(22) H(19) 0.950 no . . C(22) H(20) 0.950 no . . C(24) H(21) 0.950 no . . C(25) H(22) 0.950 no . . C(26) H(23) 0.950 no . . C(27) H(24) 0.950 no . . C(28) H(25) 0.950 no . . C(29) H(26) 0.950 no . . C(29) H(27) 0.950 no . . C(31) H(28) 0.950 no . . C(33) H(29) 0.950 no . . C(35) H(30) 0.950 no . . C(36) H(31) 0.950 no . . C(36) H(32) 0.950 no . . C(38) H(33) 0.950 no . . C(39) H(34) 0.950 no . . C(40) H(35) 0.950 no . . C(41) H(36) 0.950 no . . C(42) H(37) 0.950 no . . C(43) H(38) 0.950 no . . C(43) H(39) 0.950 no . . C(45) H(40) 0.950 no . . C(46) H(41) 0.950 no . . C(47) H(42) 0.950 no . . C(48) H(43) 0.950 no . . C(49) H(44) 0.950 no . . C(51) H(45) 0.950 no . . C(51) H(46) 0.950 no . . C(51) H(47) 0.950 no . . C(52) H(48) 0.950 no . . C(52) H(49) 0.950 no . . C(52) H(50) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I(1) Rh(1) I(2) 176.593(15) yes . . . I(1) Rh(1) O(1) 88.11(6) yes . . . I(1) Rh(1) O(2) 88.74(6) yes . . . I(1) Rh(1) C(1) 90.48(9) yes . . . I(1) Rh(1) C(4) 90.34(9) yes . . . I(2) Rh(1) O(1) 88.54(6) yes . . . I(2) Rh(1) O(2) 89.11(6) yes . . . I(2) Rh(1) C(1) 91.05(9) yes . . . I(2) Rh(1) C(4) 92.79(9) yes . . . O(1) Rh(1) O(2) 60.82(11) yes . . . O(1) Rh(1) C(1) 106.59(14) yes . . . O(1) Rh(1) C(4) 166.77(15) yes . . . O(2) Rh(1) C(1) 167.41(14) yes . . . O(2) Rh(1) C(4) 106.01(15) yes . . . C(1) Rh(1) C(4) 86.55(17) yes . . . Rh(1) O(1) C(50) 90.1(2) yes . . . Rh(1) O(2) C(50) 90.1(2) yes . . . C(11) O(3) C(15) 117.6(2) yes . . . C(13) O(4) C(22) 119.2(3) yes . . . C(32) O(5) C(36) 117.2(2) yes . . . C(34) O(6) C(43) 116.9(3) yes . . . C(1) N(1) C(2) 110.3(3) yes . . . C(1) N(1) C(8) 125.7(3) yes . . . C(2) N(1) C(8) 124.0(3) yes . . . C(1) N(2) C(3) 111.9(3) yes . . . C(1) N(2) C(7) 123.1(3) yes . . . C(3) N(2) C(7) 124.7(3) yes . . . C(4) N(3) C(5) 110.8(3) yes . . . C(4) N(3) C(29) 126.7(3) yes . . . C(5) N(3) C(29) 122.4(3) yes . . . C(4) N(4) C(6) 111.2(3) yes . . . C(4) N(4) C(7) 124.1(3) yes . . . C(6) N(4) C(7) 124.5(3) yes . . . Rh(1) C(1) N(1) 128.2(2) yes . . . Rh(1) C(1) N(2) 127.4(3) yes . . . N(1) C(1) N(2) 104.4(3) yes . . . N(1) C(2) C(3) 107.6(4) yes . . . N(2) C(3) C(2) 105.9(3) yes . . . Rh(1) C(4) N(3) 128.9(2) yes . . . Rh(1) C(4) N(4) 126.8(3) yes . . . N(3) C(4) N(4) 104.4(3) yes . . . N(3) C(5) C(6) 107.1(4) yes . . . N(4) C(6) C(5) 106.6(3) yes . . . N(2) C(7) N(4) 110.3(3) yes . . . N(1) C(8) C(9) 112.7(3) yes . . . C(8) C(9) C(10) 119.6(3) yes . . . C(8) C(9) C(14) 120.4(4) yes . . . C(10) C(9) C(14) 119.9(4) yes . . . C(9) C(10) C(11) 119.3(3) yes . . . O(3) C(11) C(10) 114.1(3) yes . . . O(3) C(11) C(12) 124.5(4) yes . . . C(10) C(11) C(12) 121.4(4) yes . . . C(11) C(12) C(13) 118.7(4) yes . . . O(4) C(13) C(12) 114.4(3) yes . . . O(4) C(13) C(14) 124.3(4) yes . . . C(12) C(13) C(14) 121.3(3) yes . . . C(9) C(14) C(13) 119.2(4) yes . . . O(3) C(15) C(16) 108.6(3) yes . . . C(15) C(16) C(17) 122.8(4) yes . . . C(15) C(16) C(21) 118.4(3) yes . . . C(17) C(16) C(21) 118.8(4) yes . . . C(16) C(17) C(18) 120.2(4) yes . . . C(17) C(18) C(19) 120.4(4) yes . . . C(18) C(19) C(20) 119.2(4) yes . . . C(19) C(20) C(21) 120.7(5) yes . . . C(16) C(21) C(20) 120.8(3) yes . . . O(4) C(22) C(23) 113.4(3) yes . . . C(22) C(23) C(24) 119.1(3) yes . . . C(22) C(23) C(28) 122.2(4) yes . . . C(24) C(23) C(28) 118.7(4) yes . . . C(23) C(24) C(25) 121.0(4) yes . . . C(24) C(25) C(26) 120.2(4) yes . . . C(25) C(26) C(27) 118.5(4) yes . . . C(26) C(27) C(28) 121.2(3) yes . . . C(23) C(28) C(27) 120.3(4) yes . . . N(3) C(29) C(30) 109.6(2) yes . . . C(29) C(30) C(31) 120.2(3) yes . . . C(29) C(30) C(35) 119.1(4) yes . . . C(31) C(30) C(35) 120.6(3) yes . . . C(30) C(31) C(32) 119.4(3) yes . . . O(5) C(32) C(31) 114.1(3) yes . . . O(5) C(32) C(33) 124.9(3) yes . . . C(31) C(32) C(33) 121.0(4) yes . . . C(32) C(33) C(34) 118.6(3) yes . . . O(6) C(34) C(33) 114.5(3) yes . . . O(6) C(34) C(35) 124.4(4) yes . . . C(33) C(34) C(35) 121.1(3) yes . . . C(30) C(35) C(34) 119.1(4) yes . . . O(5) C(36) C(37) 106.6(2) yes . . . C(36) C(37) C(38) 120.7(4) yes . . . C(36) C(37) C(42) 119.6(3) yes . . . C(38) C(37) C(42) 119.7(4) yes . . . C(37) C(38) C(39) 120.2(4) yes . . . C(38) C(39) C(40) 119.7(3) yes . . . C(39) C(40) C(41) 120.3(4) yes . . . C(40) C(41) C(42) 119.8(4) yes . . . C(37) C(42) C(41) 120.2(3) yes . . . O(6) C(43) C(44) 108.3(3) yes . . . C(43) C(44) C(45) 120.2(4) yes . . . C(43) C(44) C(49) 120.2(4) yes . . . C(45) C(44) C(49) 119.4(3) yes . . . C(44) C(45) C(46) 120.0(5) yes . . . C(45) C(46) C(47) 120.6(5) yes . . . C(46) C(47) C(48) 119.6(4) yes . . . C(47) C(48) C(49) 120.4(4) yes . . . C(44) C(49) C(48) 120.0(4) yes . . . O(1) C(50) O(2) 118.9(3) yes . . . O(1) C(50) C(51) 120.8(4) yes . . . O(2) C(50) C(51) 120.2(4) yes . . . N(5) C(53) C(52) 178.5(5) yes . . . N(1) C(2) H(1) 126.2 no . . . C(3) C(2) H(1) 126.3 no . . . N(2) C(3) H(2) 127.1 no . . . C(2) C(3) H(2) 127.1 no . . . N(3) C(5) H(3) 126.4 no . . . C(6) C(5) H(3) 126.5 no . . . N(4) C(6) H(4) 126.7 no . . . C(5) C(6) H(4) 126.7 no . . . N(2) C(7) H(5) 109.3 no . . . N(2) C(7) H(6) 109.1 no . . . N(4) C(7) H(5) 109.4 no . . . N(4) C(7) H(6) 109.2 no . . . H(5) C(7) H(6) 109.5 no . . . N(1) C(8) H(7) 108.8 no . . . N(1) C(8) H(8) 108.6 no . . . C(9) C(8) H(7) 108.6 no . . . C(9) C(8) H(8) 108.6 no . . . H(7) C(8) H(8) 109.5 no . . . C(9) C(10) H(9) 120.2 no . . . C(11) C(10) H(9) 120.4 no . . . C(11) C(12) H(10) 120.5 no . . . C(13) C(12) H(10) 120.8 no . . . C(9) C(14) H(11) 120.2 no . . . C(13) C(14) H(11) 120.6 no . . . O(3) C(15) H(12) 109.7 no . . . O(3) C(15) H(13) 109.7 no . . . C(16) C(15) H(12) 109.6 no . . . C(16) C(15) H(13) 109.9 no . . . H(12) C(15) H(13) 109.5 no . . . C(16) C(17) H(14) 119.9 no . . . C(18) C(17) H(14) 120.0 no . . . C(17) C(18) H(15) 119.7 no . . . C(19) C(18) H(15) 119.9 no . . . C(18) C(19) H(16) 120.3 no . . . C(20) C(19) H(16) 120.6 no . . . C(19) C(20) H(17) 119.5 no . . . C(21) C(20) H(17) 119.8 no . . . C(16) C(21) H(18) 119.7 no . . . C(20) C(21) H(18) 119.4 no . . . O(4) C(22) H(19) 108.4 no . . . O(4) C(22) H(20) 108.6 no . . . C(23) C(22) H(19) 108.4 no . . . C(23) C(22) H(20) 108.4 no . . . H(19) C(22) H(20) 109.5 no . . . C(23) C(24) H(21) 119.6 no . . . C(25) C(24) H(21) 119.4 no . . . C(24) C(25) H(22) 119.9 no . . . C(26) C(25) H(22) 119.9 no . . . C(25) C(26) H(23) 120.7 no . . . C(27) C(26) H(23) 120.7 no . . . C(26) C(27) H(24) 119.4 no . . . C(28) C(27) H(24) 119.4 no . . . C(23) C(28) H(25) 120.1 no . . . C(27) C(28) H(25) 119.6 no . . . N(3) C(29) H(26) 109.3 no . . . N(3) C(29) H(27) 109.5 no . . . C(30) C(29) H(26) 109.4 no . . . C(30) C(29) H(27) 109.5 no . . . H(26) C(29) H(27) 109.5 no . . . C(30) C(31) H(28) 120.2 no . . . C(32) C(31) H(28) 120.4 no . . . C(32) C(33) H(29) 120.5 no . . . C(34) C(33) H(29) 120.8 no . . . C(30) C(35) H(30) 120.5 no . . . C(34) C(35) H(30) 120.4 no . . . O(5) C(36) H(31) 110.3 no . . . O(5) C(36) H(32) 110.0 no . . . C(37) C(36) H(31) 110.5 no . . . C(37) C(36) H(32) 110.0 no . . . H(31) C(36) H(32) 109.5 no . . . C(37) C(38) H(33) 119.9 no . . . C(39) C(38) H(33) 119.8 no . . . C(38) C(39) H(34) 120.1 no . . . C(40) C(39) H(34) 120.2 no . . . C(39) C(40) H(35) 119.9 no . . . C(41) C(40) H(35) 119.8 no . . . C(40) C(41) H(36) 120.2 no . . . C(42) C(41) H(36) 120.0 no . . . C(37) C(42) H(37) 119.8 no . . . C(41) C(42) H(37) 120.0 no . . . O(6) C(43) H(38) 110.0 no . . . O(6) C(43) H(39) 109.7 no . . . C(44) C(43) H(38) 109.7 no . . . C(44) C(43) H(39) 109.8 no . . . H(38) C(43) H(39) 109.5 no . . . C(44) C(45) H(40) 120.0 no . . . C(46) C(45) H(40) 120.0 no . . . C(45) C(46) H(41) 119.7 no . . . C(47) C(46) H(41) 119.7 no . . . C(46) C(47) H(42) 120.2 no . . . C(48) C(47) H(42) 120.2 no . . . C(47) C(48) H(43) 119.7 no . . . C(49) C(48) H(43) 119.9 no . . . C(44) C(49) H(44) 120.2 no . . . C(48) C(49) H(44) 119.8 no . . . C(50) C(51) H(45) 109.5 no . . . C(50) C(51) H(46) 109.8 no . . . C(50) C(51) H(47) 109.1 no . . . H(45) C(51) H(46) 109.5 no . . . H(45) C(51) H(47) 109.5 no . . . H(46) C(51) H(47) 109.5 no . . . C(53) C(52) H(48) 109.2 no . . . C(53) C(52) H(49) 109.8 no . . . C(53) C(52) H(50) 109.4 no . . . H(48) C(52) H(49) 109.5 no . . . H(48) C(52) H(50) 109.5 no . . . H(49) C(52) H(50) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I(1) Rh(1) O(1) C(50) 88.93(19) ? . . . . I(1) Rh(1) O(2) C(50) -87.86(19) ? . . . . I(1) Rh(1) C(1) N(1) 64.4(3) ? . . . . I(1) Rh(1) C(1) N(2) -113.3(3) ? . . . . I(1) Rh(1) C(4) N(3) -63.5(3) ? . . . . I(1) Rh(1) C(4) N(4) 114.8(2) ? . . . . I(2) Rh(1) O(1) C(50) -90.47(18) ? . . . . I(2) Rh(1) O(2) C(50) 89.50(19) ? . . . . I(2) Rh(1) C(1) N(1) -112.6(3) ? . . . . I(2) Rh(1) C(1) N(2) 69.8(3) ? . . . . I(2) Rh(1) C(4) N(3) 115.1(2) ? . . . . I(2) Rh(1) C(4) N(4) -66.5(2) ? . . . . O(1) Rh(1) O(2) C(50) 0.68(18) ? . . . . O(2) Rh(1) O(1) C(50) -0.68(18) ? . . . . O(1) Rh(1) C(1) N(1) -23.8(3) ? . . . . O(1) Rh(1) C(1) N(2) 158.6(2) ? . . . . C(1) Rh(1) O(1) C(50) 178.9(2) ? . . . . O(1) Rh(1) C(4) N(3) 19.6(7) ? . . . . O(1) Rh(1) C(4) N(4) -162.0(3) ? . . . . C(4) Rh(1) O(1) C(50) 5.5(5) ? . . . . O(2) Rh(1) C(1) N(1) -22.0(7) ? . . . . O(2) Rh(1) C(1) N(2) 160.4(3) ? . . . . C(1) Rh(1) O(2) C(50) -1.3(6) ? . . . . O(2) Rh(1) C(4) N(3) 25.2(3) ? . . . . O(2) Rh(1) C(4) N(4) -156.4(2) ? . . . . C(4) Rh(1) O(2) C(50) -177.8(2) ? . . . . C(1) Rh(1) C(4) N(3) -154.0(3) ? . . . . C(1) Rh(1) C(4) N(4) 24.3(3) ? . . . . C(4) Rh(1) C(1) N(1) 154.7(3) ? . . . . C(4) Rh(1) C(1) N(2) -23.0(3) ? . . . . Rh(1) O(1) C(50) O(2) 1.2(3) ? . . . . Rh(1) O(1) C(50) C(51) -178.6(3) ? . . . . Rh(1) O(2) C(50) O(1) -1.2(3) ? . . . . Rh(1) O(2) C(50) C(51) 178.6(3) ? . . . . C(11) O(3) C(15) C(16) -172.3(3) ? . . . . C(15) O(3) C(11) C(10) 168.6(3) ? . . . . C(15) O(3) C(11) C(12) -12.1(5) ? . . . . C(13) O(4) C(22) C(23) -97.3(4) ? . . . . C(22) O(4) C(13) C(12) -168.6(3) ? . . . . C(22) O(4) C(13) C(14) 12.4(5) ? . . . . C(32) O(5) C(36) C(37) -173.5(3) ? . . . . C(36) O(5) C(32) C(31) 175.3(3) ? . . . . C(36) O(5) C(32) C(33) -4.3(5) ? . . . . C(34) O(6) C(43) C(44) 173.6(3) ? . . . . C(43) O(6) C(34) C(33) -177.4(3) ? . . . . C(43) O(6) C(34) C(35) 3.1(5) ? . . . . C(1) N(1) C(2) C(3) -0.4(4) ? . . . . C(2) N(1) C(1) Rh(1) -177.7(2) ? . . . . C(2) N(1) C(1) N(2) 0.4(3) ? . . . . C(1) N(1) C(8) C(9) 112.1(4) ? . . . . C(8) N(1) C(1) Rh(1) 1.5(5) ? . . . . C(8) N(1) C(1) N(2) 179.5(3) ? . . . . C(2) N(1) C(8) C(9) -68.9(4) ? . . . . C(8) N(1) C(2) C(3) -179.5(3) ? . . . . C(1) N(2) C(3) C(2) 0.1(3) ? . . . . C(3) N(2) C(1) Rh(1) 177.8(2) ? . . . . C(3) N(2) C(1) N(1) -0.3(4) ? . . . . C(1) N(2) C(7) N(4) 45.8(4) ? . . . . C(7) N(2) C(1) Rh(1) -8.3(5) ? . . . . C(7) N(2) C(1) N(1) 173.7(3) ? . . . . C(3) N(2) C(7) N(4) -141.0(3) ? . . . . C(7) N(2) C(3) C(2) -173.8(3) ? . . . . C(4) N(3) C(5) C(6) -0.6(4) ? . . . . C(5) N(3) C(4) Rh(1) 179.6(2) ? . . . . C(5) N(3) C(4) N(4) 1.0(3) ? . . . . C(4) N(3) C(29) C(30) -108.1(4) ? . . . . C(29) N(3) C(4) Rh(1) -4.7(4) ? . . . . C(29) N(3) C(4) N(4) 176.7(2) ? . . . . C(5) N(3) C(29) C(30) 67.1(4) ? . . . . C(29) N(3) C(5) C(6) -176.5(3) ? . . . . C(4) N(4) C(6) C(5) 0.7(4) ? . . . . C(6) N(4) C(4) Rh(1) -179.7(2) ? . . . . C(6) N(4) C(4) N(3) -1.0(3) ? . . . . C(4) N(4) C(7) N(2) -44.5(4) ? . . . . C(7) N(4) C(4) Rh(1) 5.6(4) ? . . . . C(7) N(4) C(4) N(3) -175.7(3) ? . . . . C(6) N(4) C(7) N(2) 141.5(3) ? . . . . C(7) N(4) C(6) C(5) 175.3(3) ? . . . . N(1) C(2) C(3) N(2) 0.2(3) ? . . . . N(3) C(5) C(6) N(4) -0.0(3) ? . . . . N(1) C(8) C(9) C(10) 103.1(4) ? . . . . N(1) C(8) C(9) C(14) -80.1(4) ? . . . . C(8) C(9) C(10) C(11) 173.7(3) ? . . . . C(8) C(9) C(14) C(13) -178.1(3) ? . . . . C(10) C(9) C(14) C(13) -1.3(5) ? . . . . C(14) C(9) C(10) C(11) -3.1(5) ? . . . . C(9) C(10) C(11) O(3) -176.1(3) ? . . . . C(9) C(10) C(11) C(12) 4.5(5) ? . . . . O(3) C(11) C(12) C(13) 179.2(3) ? . . . . C(10) C(11) C(12) C(13) -1.5(5) ? . . . . C(11) C(12) C(13) O(4) 178.0(3) ? . . . . C(11) C(12) C(13) C(14) -3.0(5) ? . . . . O(4) C(13) C(14) C(9) -176.7(3) ? . . . . C(12) C(13) C(14) C(9) 4.4(5) ? . . . . O(3) C(15) C(16) C(17) 16.1(5) ? . . . . O(3) C(15) C(16) C(21) -163.4(3) ? . . . . C(15) C(16) C(17) C(18) -179.1(4) ? . . . . C(15) C(16) C(21) C(20) 178.6(3) ? . . . . C(17) C(16) C(21) C(20) -0.9(6) ? . . . . C(21) C(16) C(17) C(18) 0.4(6) ? . . . . C(16) C(17) C(18) C(19) 0.7(6) ? . . . . C(17) C(18) C(19) C(20) -1.2(7) ? . . . . C(18) C(19) C(20) C(21) 0.6(6) ? . . . . C(19) C(20) C(21) C(16) 0.5(6) ? . . . . O(4) C(22) C(23) C(24) -167.8(3) ? . . . . O(4) C(22) C(23) C(28) 11.2(5) ? . . . . C(22) C(23) C(24) C(25) 178.1(4) ? . . . . C(22) C(23) C(28) C(27) -177.8(4) ? . . . . C(24) C(23) C(28) C(27) 1.2(6) ? . . . . C(28) C(23) C(24) C(25) -0.9(6) ? . . . . C(23) C(24) C(25) C(26) -0.0(7) ? . . . . C(24) C(25) C(26) C(27) 0.7(7) ? . . . . C(25) C(26) C(27) C(28) -0.5(7) ? . . . . C(26) C(27) C(28) C(23) -0.5(6) ? . . . . N(3) C(29) C(30) C(31) -94.7(4) ? . . . . N(3) C(29) C(30) C(35) 81.5(4) ? . . . . C(29) C(30) C(31) C(32) 174.1(3) ? . . . . C(29) C(30) C(35) C(34) -176.9(3) ? . . . . C(31) C(30) C(35) C(34) -0.6(6) ? . . . . C(35) C(30) C(31) C(32) -2.1(6) ? . . . . C(30) C(31) C(32) O(5) -175.8(3) ? . . . . C(30) C(31) C(32) C(33) 3.9(6) ? . . . . O(5) C(32) C(33) C(34) 176.8(3) ? . . . . C(31) C(32) C(33) C(34) -2.8(6) ? . . . . C(32) C(33) C(34) O(6) -179.5(3) ? . . . . C(32) C(33) C(34) C(35) -0.0(5) ? . . . . O(6) C(34) C(35) C(30) -178.9(3) ? . . . . C(33) C(34) C(35) C(30) 1.7(6) ? . . . . O(5) C(36) C(37) C(38) 92.0(4) ? . . . . O(5) C(36) C(37) C(42) -86.4(4) ? . . . . C(36) C(37) C(38) C(39) -178.4(3) ? . . . . C(36) C(37) C(42) C(41) 177.2(3) ? . . . . C(38) C(37) C(42) C(41) -1.2(5) ? . . . . C(42) C(37) C(38) C(39) -0.0(5) ? . . . . C(37) C(38) C(39) C(40) 1.0(5) ? . . . . C(38) C(39) C(40) C(41) -0.7(6) ? . . . . C(39) C(40) C(41) C(42) -0.5(6) ? . . . . C(40) C(41) C(42) C(37) 1.5(5) ? . . . . O(6) C(43) C(44) C(45) 146.3(3) ? . . . . O(6) C(43) C(44) C(49) -39.0(4) ? . . . . C(43) C(44) C(45) C(46) 176.1(3) ? . . . . C(43) C(44) C(49) C(48) -176.1(3) ? . . . . C(45) C(44) C(49) C(48) -1.3(5) ? . . . . C(49) C(44) C(45) C(46) 1.3(6) ? . . . . C(44) C(45) C(46) C(47) -1.1(6) ? . . . . C(45) C(46) C(47) C(48) 0.9(7) ? . . . . C(46) C(47) C(48) C(49) -0.9(6) ? . . . . C(47) C(48) C(49) C(44) 1.1(6) ? . . . . #============================================================================== data_3d _database_code_depnum_ccdc_archive 'CCDC 633259' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C11 H15 I2 N4 O2 Rh ' _chemical_formula_moiety 'C11 H15 I2 N4 O2 Rh ' _chemical_formula_weight 591.98 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 +X,-Y,1/2+Z 3 1/2+X,1/2+Y,+Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.685(2) _cell_length_b 13.321(3) _cell_length_c 12.691(3) _cell_angle_alpha 90.0000 _cell_angle_beta 94.340(2) _cell_angle_gamma 90.0000 _cell_volume 1632.6(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2910 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.408 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104.00 _exptl_absorpt_coefficient_mu 4.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.240 _exptl_absorpt_correction_T_max 0.380 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 5739 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 2705 _reflns_number_gt 2704 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0591 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2705 _refine_ls_number_parameters 197 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 0.2000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.33 _refine_diff_density_min -0.86 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 878 Friedel Pairs' _refine_ls_abs_structure_Flack 0.222(16) 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) ; N N 0.006 0.003 ; 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) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.88507(5) 0.76886(2) 0.53822(3) 0.01328(6) Uani 1.00 1 d . . . I(2) I 0.37791(5) 0.88562(2) 0.40382(4) 0.01308(6) Uani 1.00 1 d . . . Rh(1) Rh 0.63290(5) 0.82597(2) 0.46844(4) 0.00717(6) Uani 1.00 1 d . . . O(1) O 0.6790(3) 0.7932(2) 0.3051(2) 0.0126(6) Uani 1.00 1 d . . . O(2) O 0.5914(2) 0.6769(2) 0.4032(2) 0.0111(6) Uani 1.00 1 d . . . N(1) N 0.5746(3) 0.7379(2) 0.6774(2) 0.0118(7) Uani 1.00 1 d . . . N(2) N 0.5544(3) 0.8985(2) 0.6779(2) 0.0113(7) Uani 1.00 1 d . . . N(3) N 0.7791(3) 1.0218(2) 0.4451(2) 0.0126(7) Uani 1.00 1 d . . . N(4) N 0.6493(3) 1.0270(2) 0.5748(2) 0.0104(7) Uani 1.00 1 d . . . C(1) C 0.5835(3) 0.8204(3) 0.6154(2) 0.0119(8) Uani 1.00 1 d . . . C(2) C 0.5410(4) 0.7677(3) 0.7778(2) 0.0151(9) Uani 1.00 1 d . . . C(3) C 0.5284(4) 0.8651(3) 0.7787(2) 0.0153(9) Uani 1.00 1 d . . . C(4) C 0.6045(4) 0.6343(3) 0.6494(2) 0.0145(9) Uani 1.00 1 d . . . C(5) C 0.5407(4) 1.0023(3) 0.6415(2) 0.0135(8) Uani 1.00 1 d . . . C(6) C 0.6897(4) 0.9661(2) 0.4956(2) 0.0119(8) Uani 1.00 1 d . . . C(7) C 0.7946(4) 1.1164(2) 0.4899(3) 0.0136(8) Uani 1.00 1 d . . . C(8) C 0.7144(4) 1.1196(2) 0.5702(2) 0.0136(8) Uani 1.00 1 d . . . C(9) C 0.8543(4) 0.9910(3) 0.3552(3) 0.0164(9) Uani 1.00 1 d . . . C(10) C 0.6442(4) 0.7015(2) 0.3190(3) 0.0127(8) Uani 1.00 1 d . . . C(11) C 0.6647(4) 0.6243(3) 0.2359(3) 0.0161(9) Uani 1.00 1 d . . . H(1) H 0.5289 0.7240 0.8356 0.018 Uiso 1.00 1 c R . . H(2) H 0.5066 0.9054 0.8369 0.019 Uiso 1.00 1 c R . . H(3) H 0.5226 0.6035 0.6187 0.018 Uiso 1.00 1 c R . . H(4) H 0.6371 0.5982 0.7109 0.018 Uiso 1.00 1 c R . . H(5) H 0.6734 0.6338 0.5999 0.018 Uiso 1.00 1 c R . . H(6) H 0.4536 1.0103 0.6027 0.016 Uiso 1.00 1 c R . . H(7) H 0.5459 1.0460 0.7008 0.016 Uiso 1.00 1 c R . . H(8) H 0.8519 1.1689 0.4674 0.016 Uiso 1.00 1 c R . . H(9) H 0.7029 1.1748 0.6161 0.016 Uiso 1.00 1 c R . . H(10) H 0.9406 0.9627 0.3801 0.020 Uiso 1.00 1 c R . . H(11) H 0.8699 1.0479 0.3125 0.020 Uiso 1.00 1 c R . . H(12) H 0.8017 0.9426 0.3145 0.020 Uiso 1.00 1 c R . . H(13) H 0.5842 0.6212 0.1883 0.019 Uiso 1.00 1 c R . . H(14) H 0.6809 0.5605 0.2678 0.019 Uiso 1.00 1 c R . . H(15) H 0.7421 0.6427 0.1984 0.019 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.01036(12) 0.01693(14) 0.01267(12) 0.00245(9) 0.00156(8) 0.00092(9) I(2) 0.01082(12) 0.01180(13) 0.01624(12) -0.00116(9) -0.00154(8) 0.00398(8) Rh(1) 0.00869(13) 0.00619(14) 0.00678(12) -0.00125(9) 0.00159(9) 0.00049(8) O(1) 0.0198(14) 0.0090(13) 0.0093(11) -0.0021(10) 0.0039(10) -0.0010(9) O(2) 0.0130(13) 0.0062(13) 0.0140(11) -0.0019(9) -0.0007(10) -0.0010(9) N(1) 0.0121(15) 0.0141(17) 0.0097(14) 0.0002(11) 0.0040(11) 0.0015(11) N(2) 0.0145(16) 0.0157(17) 0.0045(12) -0.0005(12) 0.0065(11) 0.0033(10) N(3) 0.0117(15) 0.0114(16) 0.0145(13) -0.0017(11) 0.0003(12) -0.0019(11) N(4) 0.0119(15) 0.0105(16) 0.0093(12) -0.0012(11) 0.0036(11) -0.0036(10) C(1) 0.0099(16) 0.0150(19) 0.0114(15) -0.0014(13) 0.0048(12) 0.0008(13) C(2) 0.0155(19) 0.024(2) 0.0066(16) 0.0019(14) 0.0046(13) 0.0019(13) C(3) 0.0153(19) 0.027(2) 0.0040(14) -0.0033(15) 0.0027(12) 0.0002(13) C(4) 0.0171(19) 0.0129(18) 0.0133(17) -0.0013(14) -0.0007(14) 0.0056(13) C(5) 0.0131(17) 0.0118(18) 0.0161(16) 0.0008(13) 0.0039(13) 0.0048(12) C(6) 0.0190(19) 0.0072(16) 0.0099(15) 0.0018(14) 0.0041(13) 0.0001(12) C(7) 0.0167(18) 0.0085(17) 0.0153(16) -0.0008(14) -0.0008(14) 0.0011(12) C(8) 0.022(2) 0.0065(16) 0.0127(16) -0.0048(13) 0.0016(14) -0.0036(11) C(9) 0.0165(19) 0.019(2) 0.0148(16) -0.0060(15) 0.0083(14) 0.0008(14) C(10) 0.0122(18) 0.0106(18) 0.0147(16) -0.0007(14) -0.0027(14) 0.0004(13) C(11) 0.0176(19) 0.0107(18) 0.0196(17) 0.0001(14) -0.0013(14) -0.0012(14) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Rh(1) 2.6459(6) yes . . I(2) Rh(1) 2.6640(6) yes . . Rh(1) O(1) 2.196(2) yes . . Rh(1) O(2) 2.177(2) yes . . Rh(1) C(1) 1.961(3) yes . . Rh(1) C(6) 1.969(3) yes . . O(1) C(10) 1.283(4) yes . . O(2) C(10) 1.263(4) yes . . N(1) C(1) 1.358(5) yes . . N(1) C(2) 1.396(5) yes . . N(1) C(4) 1.460(5) yes . . N(2) C(1) 1.351(5) yes . . N(2) C(3) 1.396(4) yes . . N(2) C(5) 1.460(5) yes . . N(3) C(6) 1.340(5) yes . . N(3) C(7) 1.386(5) yes . . N(3) C(9) 1.459(5) yes . . N(4) C(5) 1.437(5) yes . . N(4) C(6) 1.371(4) yes . . N(4) C(8) 1.388(5) yes . . C(2) C(3) 1.304(6) yes . . C(7) C(8) 1.329(5) yes . . C(10) C(11) 1.497(5) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(4) H(4) 0.950 no . . C(4) H(5) 0.950 no . . C(5) H(6) 0.950 no . . C(5) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(9) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(11) H(13) 0.950 no . . C(11) H(14) 0.950 no . . C(11) H(15) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I(1) Rh(1) I(2) 178.31(2) yes . . . I(1) Rh(1) O(1) 90.59(7) yes . . . I(1) Rh(1) O(2) 90.25(7) yes . . . I(1) Rh(1) C(1) 87.51(11) yes . . . I(1) Rh(1) C(6) 88.60(11) yes . . . I(2) Rh(1) O(1) 91.07(8) yes . . . I(2) Rh(1) O(2) 90.84(7) yes . . . I(2) Rh(1) C(1) 90.95(11) yes . . . I(2) Rh(1) C(6) 90.64(11) yes . . . O(1) Rh(1) O(2) 60.34(10) yes . . . O(1) Rh(1) C(1) 166.21(14) yes . . . O(1) Rh(1) C(6) 106.24(12) yes . . . O(2) Rh(1) C(1) 105.99(14) yes . . . O(2) Rh(1) C(6) 166.52(13) yes . . . C(1) Rh(1) C(6) 87.37(15) yes . . . Rh(1) O(1) C(10) 89.2(2) yes . . . Rh(1) O(2) C(10) 90.5(2) yes . . . C(1) N(1) C(2) 109.2(3) yes . . . C(1) N(1) C(4) 127.0(3) yes . . . C(2) N(1) C(4) 123.7(3) yes . . . C(1) N(2) C(3) 110.7(3) yes . . . C(1) N(2) C(5) 124.1(3) yes . . . C(3) N(2) C(5) 125.0(3) yes . . . C(6) N(3) C(7) 111.2(3) yes . . . C(6) N(3) C(9) 126.7(3) yes . . . C(7) N(3) C(9) 122.1(3) yes . . . C(5) N(4) C(6) 123.9(3) yes . . . C(5) N(4) C(8) 125.7(3) yes . . . C(6) N(4) C(8) 109.9(3) yes . . . Rh(1) C(1) N(1) 127.7(2) yes . . . Rh(1) C(1) N(2) 127.3(2) yes . . . N(1) C(1) N(2) 104.9(3) yes . . . N(1) C(2) C(3) 108.6(3) yes . . . N(2) C(3) C(2) 106.6(3) yes . . . N(2) C(5) N(4) 110.5(3) yes . . . Rh(1) C(6) N(3) 128.5(2) yes . . . Rh(1) C(6) N(4) 126.7(2) yes . . . N(3) C(6) N(4) 104.7(3) yes . . . N(3) C(7) C(8) 107.0(3) yes . . . N(4) C(8) C(7) 107.3(3) yes . . . O(1) C(10) O(2) 119.4(3) yes . . . O(1) C(10) C(11) 120.5(3) yes . . . O(2) C(10) C(11) 120.1(3) yes . . . N(1) C(2) H(1) 125.5 no . . . C(3) C(2) H(1) 125.8 no . . . N(2) C(3) H(2) 126.8 no . . . C(2) C(3) H(2) 126.6 no . . . N(1) C(4) H(3) 109.4 no . . . N(1) C(4) H(4) 109.8 no . . . N(1) C(4) H(5) 109.2 no . . . H(3) C(4) H(4) 109.5 no . . . H(3) C(4) H(5) 109.5 no . . . H(4) C(4) H(5) 109.5 no . . . N(2) C(5) H(6) 109.1 no . . . N(2) C(5) H(7) 109.4 no . . . N(4) C(5) H(6) 109.2 no . . . N(4) C(5) H(7) 109.2 no . . . H(6) C(5) H(7) 109.5 no . . . N(3) C(7) H(8) 126.4 no . . . C(8) C(7) H(8) 126.6 no . . . N(4) C(8) H(9) 126.0 no . . . C(7) C(8) H(9) 126.7 no . . . N(3) C(9) H(10) 109.3 no . . . N(3) C(9) H(11) 109.4 no . . . N(3) C(9) H(12) 109.7 no . . . H(10) C(9) H(11) 109.5 no . . . H(10) C(9) H(12) 109.5 no . . . H(11) C(9) H(12) 109.5 no . . . C(10) C(11) H(13) 109.3 no . . . C(10) C(11) H(14) 109.9 no . . . C(10) C(11) H(15) 109.1 no . . . H(13) C(11) H(14) 109.5 no . . . H(13) C(11) H(15) 109.5 no . . . H(14) C(11) H(15) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I(1) Rh(1) O(1) C(10) 85.8(2) ? . . . . I(1) Rh(1) O(2) C(10) -86.3(2) ? . . . . I(1) Rh(1) C(1) N(1) -67.4(3) ? . . . . I(1) Rh(1) C(1) N(2) 110.6(3) ? . . . . I(1) Rh(1) C(6) N(3) 69.1(3) ? . . . . I(1) Rh(1) C(6) N(4) -108.0(3) ? . . . . I(2) Rh(1) O(1) C(10) -94.5(2) ? . . . . I(2) Rh(1) O(2) C(10) 95.0(2) ? . . . . I(2) Rh(1) C(1) N(1) 113.2(3) ? . . . . I(2) Rh(1) C(1) N(2) -68.7(3) ? . . . . I(2) Rh(1) C(6) N(3) -112.4(3) ? . . . . I(2) Rh(1) C(6) N(4) 70.5(3) ? . . . . O(1) Rh(1) O(2) C(10) 4.3(2) ? . . . . O(2) Rh(1) O(1) C(10) -4.2(2) ? . . . . O(1) Rh(1) C(1) N(1) 14.9(8) ? . . . . O(1) Rh(1) C(1) N(2) -167.1(4) ? . . . . C(1) Rh(1) O(1) C(10) 3.8(6) ? . . . . O(1) Rh(1) C(6) N(3) -21.1(3) ? . . . . O(1) Rh(1) C(6) N(4) 161.8(3) ? . . . . C(6) Rh(1) O(1) C(10) 174.5(2) ? . . . . O(2) Rh(1) C(1) N(1) 22.1(3) ? . . . . O(2) Rh(1) C(1) N(2) -159.9(3) ? . . . . C(1) Rh(1) O(2) C(10) -173.8(2) ? . . . . O(2) Rh(1) C(6) N(3) -16.1(8) ? . . . . O(2) Rh(1) C(6) N(4) 166.8(4) ? . . . . C(6) Rh(1) O(2) C(10) -1.3(6) ? . . . . C(1) Rh(1) C(6) N(3) 156.7(3) ? . . . . C(1) Rh(1) C(6) N(4) -20.4(3) ? . . . . C(6) Rh(1) C(1) N(1) -156.2(3) ? . . . . C(6) Rh(1) C(1) N(2) 21.9(3) ? . . . . Rh(1) O(1) C(10) O(2) 7.2(3) ? . . . . Rh(1) O(1) C(10) C(11) -173.3(3) ? . . . . Rh(1) O(2) C(10) O(1) -7.3(3) ? . . . . Rh(1) O(2) C(10) C(11) 173.2(3) ? . . . . C(1) N(1) C(2) C(3) 0.4(4) ? . . . . C(2) N(1) C(1) Rh(1) 177.9(2) ? . . . . C(2) N(1) C(1) N(2) -0.4(4) ? . . . . C(4) N(1) C(1) Rh(1) 2.1(5) ? . . . . C(4) N(1) C(1) N(2) -176.2(3) ? . . . . C(4) N(1) C(2) C(3) 176.3(3) ? . . . . C(1) N(2) C(3) C(2) -0.1(3) ? . . . . C(3) N(2) C(1) Rh(1) -178.0(2) ? . . . . C(3) N(2) C(1) N(1) 0.3(4) ? . . . . C(1) N(2) C(5) N(4) -43.7(4) ? . . . . C(5) N(2) C(1) Rh(1) 6.9(5) ? . . . . C(5) N(2) C(1) N(1) -174.8(3) ? . . . . C(3) N(2) C(5) N(4) 141.8(3) ? . . . . C(5) N(2) C(3) C(2) 174.9(3) ? . . . . C(6) N(3) C(7) C(8) 0.5(4) ? . . . . C(7) N(3) C(6) Rh(1) -178.2(2) ? . . . . C(7) N(3) C(6) N(4) -0.6(4) ? . . . . C(9) N(3) C(6) Rh(1) 1.2(5) ? . . . . C(9) N(3) C(6) N(4) 178.8(3) ? . . . . C(9) N(3) C(7) C(8) -179.0(3) ? . . . . C(5) N(4) C(6) Rh(1) -10.1(5) ? . . . . C(5) N(4) C(6) N(3) 172.3(3) ? . . . . C(6) N(4) C(5) N(2) 45.2(4) ? . . . . C(5) N(4) C(8) C(7) -171.8(3) ? . . . . C(8) N(4) C(5) N(2) -144.4(3) ? . . . . C(6) N(4) C(8) C(7) -0.3(4) ? . . . . C(8) N(4) C(6) Rh(1) 178.2(2) ? . . . . C(8) N(4) C(6) N(3) 0.5(4) ? . . . . N(1) C(2) C(3) N(2) -0.1(3) ? . . . . N(3) C(7) C(8) N(4) -0.1(3) ? . . . . #============================================================================== # End of CIF #==============================================================================