# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1720 #------------------------------------------------------------------------------ data_rh-2bpbd-bf4.cif #(1a) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C25 H26 B F4 N2 O Rh ' _chemical_formula_moiety '?' _chemical_formula_weight 560.20 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 14.38(5) _cell_length_b 10.14(4) _cell_length_c 17.62(2) _cell_angle_alpha 90 _cell_angle_beta 95.24(3) _cell_angle_gamma 90 _cell_volume 2557(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5858 _cell_measurement_theta_min ? _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_reflns_number 5858 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max ? _diffrn_measured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 4698 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1430 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5839 _refine_ls_number_parameters 307 _refine_ls_goodness_of_fit_ref 1.714 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0030 _refine_diff_density_max 0.97 _refine_diff_density_min -0.63 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rh' 'Rh' -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh(1) Rh 0.14895(2) 0.22887(3) 0.90039(2) 0.03758(9) Uani 1.00 d . . . F(1) F 0.5527(3) 0.1255(5) 0.2044(3) 0.150(2) Uani 1.00 d . . . F(2) F 0.6807(4) 0.000(1) 0.2084(6) 0.290(5) Uani 1.00 d . . . F(3) F 0.5559(7) -0.0771(7) 0.2076(6) 0.259(5) Uani 1.00 d . . . F(4) F 0.6003(9) 0.039(1) 0.1132(4) 0.342(6) Uani 1.00 d . . . O(1) O 0.7502(9) 0.177(2) 0.4618(10) 0.309(8) Uani 1.00 d . . . N(1) N 0.2296(2) 0.3828(3) 0.8596(2) 0.0427(8) Uani 1.00 d . . . N(2) N 0.2362(2) 0.2437(3) 1.0030(2) 0.0498(9) Uani 1.00 d . . . C(1) C 0.3114(3) 0.3526(4) 0.8323(3) 0.056(1) Uani 1.00 d . . . C(2) C 0.3712(4) 0.4463(6) 0.8078(3) 0.075(2) Uani 1.00 d . . . C(3) C 0.3468(4) 0.5735(6) 0.8108(4) 0.082(2) Uani 1.00 d . . . C(4) C 0.2619(4) 0.6084(5) 0.8400(4) 0.078(2) Uani 1.00 d . . . C(5) C 0.2066(3) 0.5100(4) 0.8630(2) 0.049(1) Uani 1.00 d . . . C(6) C 0.1164(3) 0.5403(4) 0.8887(2) 0.051(1) Uani 1.00 d . . . C(7) C 0.0418(3) 0.5702(4) 0.9055(2) 0.051(1) Uani 1.00 d . . . C(8) C -0.0468(3) 0.6059(4) 0.9209(2) 0.052(1) Uani 1.00 d . . . C(9) C -0.1233(3) 0.6394(5) 0.9320(2) 0.055(1) Uani 1.00 d . . . C(10) C 0.2173(3) 0.3116(5) 1.0653(2) 0.051(1) Uani 1.00 d . . . C(11) C 0.2818(3) 0.3315(6) 1.1260(3) 0.070(2) Uani 1.00 d . . . C(12) C 0.3694(4) 0.2731(7) 1.1253(4) 0.081(2) Uani 1.00 d . . . C(13) C 0.3870(3) 0.1989(7) 1.0642(3) 0.084(2) Uani 1.00 d . . . C(14) C 0.3206(3) 0.1857(6) 1.0044(3) 0.069(1) Uani 1.00 d . . . C(15) C 0.0443(4) 0.2518(4) 0.8087(3) 0.057(1) Uani 1.00 d . . . C(16) C -0.0502(4) 0.2221(7) 0.8360(4) 0.094(2) Uani 1.00 d . . . C(17) C -0.0491(3) 0.1359(6) 0.9045(4) 0.086(2) Uani 1.00 d . . . C(18) C 0.0424(3) 0.1174(4) 0.9467(2) 0.054(1) Uani 1.00 d . . . C(19) C 0.1111(3) 0.0320(4) 0.9263(3) 0.063(1) Uani 1.00 d . . . C(20) C 0.1069(6) -0.0490(5) 0.8548(5) 0.114(3) Uani 1.00 d . . . C(21) C 0.0946(5) 0.0190(5) 0.7835(4) 0.090(2) Uani 1.00 d . . . C(22) C 0.1092(3) 0.1643(5) 0.7873(2) 0.057(1) Uani 1.00 d . . . C(23) C 0.660(2) 0.330(3) 0.391(2) 0.38(2) Uani 1.00 d . . . C(24) C 0.6778(9) 0.229(2) 0.4437(8) 0.225(8) Uani 1.00 d . . . C(25) C 0.594(1) 0.135(2) 0.458(1) 0.29(1) Uani 1.00 d . . . B(1) B 0.6006(5) 0.0283(7) 0.1841(4) 0.085(2) Uani 1.00 d . . . H(1) H 0.3292 0.2583 0.8312 0.0657 Uiso 1.00 calc . . . H(2) H 0.4356 0.4159 0.7843 0.0657 Uiso 1.00 calc . . . H(3) H 0.3747 0.6446 0.7847 0.0657 Uiso 1.00 calc . . . H(4) H 0.2432 0.6996 0.8520 0.0657 Uiso 1.00 calc . . . H(5) H 0.2671 0.3964 1.1719 0.0657 Uiso 1.00 calc . . . H(6) H 0.4212 0.2604 1.1707 0.0657 Uiso 1.00 calc . . . H(7) H 0.4602 0.1703 1.0604 0.0657 Uiso 1.00 calc . . . H(8) H 0.3296 0.1332 0.9581 0.0657 Uiso 1.00 calc . . . H(9) H 0.0466 0.3517 0.7927 0.0657 Uiso 1.00 calc . . . H(10) H -0.0861 0.1754 0.7942 0.0657 Uiso 1.00 calc . . . H(11) H -0.1076 0.2469 0.8115 0.0657 Uiso 1.00 calc . . . H(12) H -0.0629 0.0532 0.8696 0.0657 Uiso 1.00 calc . . . H(13) H -0.1032 0.1178 0.9282 0.0657 Uiso 1.00 calc . . . H(14) H 0.0441 0.1416 1.0016 0.0657 Uiso 1.00 calc . . . H(15) H 0.1723 -0.0085 0.9757 0.0657 Uiso 1.00 calc . . . H(16) H 0.1598 -0.1069 0.8474 0.0657 Uiso 1.00 calc . . . H(17) H 0.0866 -0.1343 0.8692 0.0657 Uiso 1.00 calc . . . H(18) H 0.1314 -0.0249 0.7450 0.0657 Uiso 1.00 calc . . . H(19) H 0.0221 -0.0049 0.7624 0.0657 Uiso 1.00 calc . . . H(20) H 0.1652 0.2041 0.7572 0.0657 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0365(2) 0.0356(2) 0.0414(2) 0.0028(1) 0.0074(1) 0.0023(1) F(1) 0.136(4) 0.112(4) 0.203(5) 0.038(3) 0.032(3) -0.025(3) F(2) 0.092(4) 0.43(1) 0.35(1) 0.093(6) 0.039(5) 0.21(1) F(3) 0.33(1) 0.117(5) 0.34(1) -0.020(6) 0.063(9) 0.005(6) F(4) 0.44(1) 0.49(2) 0.115(5) 0.27(1) 0.097(7) 0.052(7) O(1) 0.152(9) 0.44(2) 0.34(2) -0.01(1) 0.05(1) 0.07(2) N(1) 0.037(2) 0.039(2) 0.053(2) 0.001(1) 0.011(1) 0.001(1) N(2) 0.036(2) 0.069(2) 0.045(2) 0.011(1) 0.007(1) -0.001(1) C(1) 0.042(2) 0.051(2) 0.080(3) 0.002(2) 0.025(2) -0.004(2) C(2) 0.056(3) 0.074(3) 0.101(4) 0.000(2) 0.034(3) -0.006(3) C(3) 0.072(3) 0.071(3) 0.108(4) -0.017(3) 0.033(3) 0.010(3) C(4) 0.062(3) 0.046(2) 0.132(5) -0.006(2) 0.032(3) 0.002(3) C(5) 0.041(2) 0.043(2) 0.064(2) 0.003(2) 0.013(2) 0.000(2) C(6) 0.048(2) 0.045(2) 0.062(2) 0.006(2) 0.010(2) -0.001(2) C(7) 0.048(2) 0.047(2) 0.060(2) 0.003(2) 0.014(2) -0.004(2) C(8) 0.050(2) 0.054(2) 0.053(2) 0.008(2) 0.009(2) -0.005(2) C(9) 0.054(2) 0.069(3) 0.043(2) 0.009(2) 0.009(2) -0.005(2) C(10) 0.039(2) 0.071(3) 0.042(2) 0.004(2) 0.007(2) -0.001(2) C(11) 0.056(3) 0.105(4) 0.048(2) 0.002(3) 0.004(2) -0.002(2) C(12) 0.049(3) 0.128(5) 0.063(3) 0.004(3) -0.007(2) 0.014(3) C(13) 0.041(3) 0.136(5) 0.076(3) 0.025(3) 0.005(2) 0.019(3) C(14) 0.050(3) 0.096(3) 0.062(3) 0.029(3) 0.012(2) 0.001(3) C(15) 0.054(3) 0.063(3) 0.052(2) -0.001(2) -0.008(2) 0.015(2) C(16) 0.039(3) 0.138(6) 0.100(4) -0.008(3) -0.011(3) 0.052(4) C(17) 0.046(3) 0.104(4) 0.105(4) -0.019(3) -0.002(3) 0.038(3) C(18) 0.055(2) 0.051(2) 0.059(2) -0.005(2) 0.016(2) 0.013(2) C(19) 0.069(3) 0.037(2) 0.086(3) -0.002(2) 0.016(2) 0.019(2) C(20) 0.175(7) 0.030(2) 0.147(6) -0.010(3) 0.066(6) -0.011(3) C(21) 0.116(5) 0.055(3) 0.096(4) -0.017(3) -0.006(4) -0.028(3) C(22) 0.063(3) 0.061(3) 0.046(2) -0.014(2) -0.002(2) -0.008(2) C(23) 0.44(4) 0.31(3) 0.41(4) 0.17(3) 0.13(3) 0.10(3) C(24) 0.080(7) 0.46(3) 0.131(10) 0.04(1) -0.009(7) -0.03(1) C(25) 0.17(1) 0.36(3) 0.37(3) -0.08(2) 0.10(2) -0.10(2) B(1) 0.082(4) 0.079(4) 0.097(5) 0.044(4) 0.032(4) 0.022(4) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) N(1) 2.109(4) . . yes Rh(1) N(2) 2.110(4) . . yes Rh(1) C(15) 2.117(6) . . yes Rh(1) C(18) 2.125(5) . . yes Rh(1) C(19) 2.129(4) . . yes Rh(1) C(22) 2.125(4) . . yes F(1) B(1) 1.273(7) . . yes F(2) B(1) 1.225(9) . . yes F(3) B(1) 1.33(1) . . yes F(4) B(1) 1.254(9) . . yes O(1) C(24) 1.18(2) . . yes N(1) C(1) 1.346(6) . . yes N(1) C(5) 1.335(5) . . yes N(2) C(10) 1.344(5) . . yes N(2) C(14) 1.346(6) . . yes C(1) C(2) 1.377(7) . . yes C(1) H(1) 0.991 . . no C(2) C(3) 1.339(8) . . yes C(2) H(2) 1.091 . . no C(3) C(4) 1.411(8) . . yes C(3) H(3) 0.963 . . no C(4) C(5) 1.360(6) . . yes C(4) H(4) 0.991 . . no C(5) C(6) 1.445(7) . . yes C(6) C(7) 1.178(6) . . yes C(7) C(8) 1.376(7) . . yes C(8) C(9) 1.183(6) . . yes C(9) C(10) 1.445(7) . 3_567 yes C(10) C(11) 1.364(6) . . yes C(11) C(12) 1.393(8) . . yes C(11) H(5) 1.080 . . no C(12) C(13) 1.355(9) . . yes C(12) H(6) 1.051 . . no C(13) C(14) 1.362(8) . . yes C(13) H(7) 1.100 . . no C(14) H(8) 0.993 . . no C(15) C(16) 1.512(9) . . yes C(15) C(22) 1.365(7) . . yes C(15) H(9) 1.053 . . no C(16) C(17) 1.489(8) . . yes C(16) H(10) 0.983 . . no C(16) H(11) 0.931 . . no C(17) C(18) 1.463(8) . . yes C(17) H(12) 1.048 . . no C(17) H(13) 0.933 . . no C(18) C(19) 1.385(6) . . yes C(18) H(14) 0.997 . . no C(19) C(20) 1.499(8) . . yes C(19) H(15) 1.250 . . no C(20) C(21) 1.430(10) . . yes C(20) H(16) 0.980 . . no C(20) H(17) 0.954 . . no C(21) C(22) 1.488(7) . . yes C(21) H(18) 1.002 . . no C(21) H(19) 1.101 . . no C(22) H(20) 1.083 . . no C(23) C(24) 1.39(3) . . yes C(24) C(25) 1.57(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Rh(1) N(2) 86.4(2) . 1_555 1_555 yes N(1) Rh(1) C(15) 91.9(2) . 1_555 1_555 yes N(1) Rh(1) C(18) 164.2(1) . 1_555 1_555 yes N(1) Rh(1) C(19) 157.8(2) . 1_555 1_555 yes N(1) Rh(1) C(22) 91.0(2) . 1_555 1_555 yes N(2) Rh(1) C(15) 166.3(2) . 1_555 1_555 yes N(2) Rh(1) C(18) 95.8(2) . 1_555 1_555 yes N(2) Rh(1) C(19) 91.5(2) . 1_555 1_555 yes N(2) Rh(1) C(22) 156.0(2) . 1_555 1_555 yes C(15) Rh(1) C(18) 82.2(2) . 1_555 1_555 yes C(15) Rh(1) C(19) 95.1(2) . 1_555 1_555 yes C(15) Rh(1) C(22) 37.6(2) . 1_555 1_555 yes C(18) Rh(1) C(19) 38.0(2) . 1_555 1_555 yes C(18) Rh(1) C(22) 93.1(2) . 1_555 1_555 yes C(19) Rh(1) C(22) 81.9(2) . 1_555 1_555 yes Rh(1) N(1) C(1) 118.6(3) . 1_555 1_555 yes Rh(1) N(1) C(5) 123.6(3) . 1_555 1_555 yes C(1) N(1) C(5) 117.6(3) . 1_555 1_555 yes Rh(1) N(2) C(10) 126.0(3) . 1_555 1_555 yes Rh(1) N(2) C(14) 116.6(3) . 1_555 1_555 yes C(10) N(2) C(14) 117.3(4) . 1_555 1_555 yes N(1) C(1) C(2) 123.1(4) . 1_555 1_555 yes N(1) C(1) H(1) 117.5 . 1_555 1_555 no C(2) C(1) H(1) 119.4 . 1_555 1_555 no C(1) C(2) C(3) 118.5(5) . 1_555 1_555 yes C(1) C(2) H(2) 119.9 . 1_555 1_555 no C(3) C(2) H(2) 121.5 . 1_555 1_555 no C(2) C(3) C(4) 119.7(4) . 1_555 1_555 yes C(2) C(3) H(3) 125.4 . 1_555 1_555 no C(4) C(3) H(3) 113.5 . 1_555 1_555 no C(3) C(4) C(5) 118.2(4) . 1_555 1_555 yes C(3) C(4) H(4) 124.8 . 1_555 1_555 no C(5) C(4) H(4) 116.3 . 1_555 1_555 no N(1) C(5) C(4) 122.8(4) . 1_555 1_555 yes N(1) C(5) C(6) 116.9(3) . 1_555 1_555 yes C(4) C(5) C(6) 120.2(4) . 1_555 1_555 yes C(5) C(6) C(7) 175.6(5) . 1_555 1_555 yes C(6) C(7) C(8) 176.8(5) . 1_555 1_555 yes C(7) C(8) C(9) 177.7(5) . 1_555 1_555 yes C(8) C(9) C(10) 171.8(4) . 1_555 3_567 yes N(2) C(10) C(9) 117.5(4) . 1_555 3_567 yes N(2) C(10) C(11) 122.8(4) . 1_555 1_555 yes C(9) C(10) C(11) 119.6(4) . 3_567 1_555 yes C(10) C(11) C(12) 118.8(5) . 1_555 1_555 yes C(10) C(11) H(5) 120.8 . 1_555 1_555 no C(12) C(11) H(5) 120.4 . 1_555 1_555 no C(11) C(12) C(13) 118.5(5) . 1_555 1_555 yes C(11) C(12) H(6) 128.6 . 1_555 1_555 no C(13) C(12) H(6) 111.5 . 1_555 1_555 no C(12) C(13) C(14) 120.0(5) . 1_555 1_555 yes C(12) C(13) H(7) 116.4 . 1_555 1_555 no C(14) C(13) H(7) 122.2 . 1_555 1_555 no N(2) C(14) C(13) 122.5(5) . 1_555 1_555 yes N(2) C(14) H(8) 113.9 . 1_555 1_555 no C(13) C(14) H(8) 123.6 . 1_555 1_555 no Rh(1) C(15) C(16) 109.4(4) . 1_555 1_555 yes Rh(1) C(15) C(22) 71.6(3) . 1_555 1_555 yes Rh(1) C(15) H(9) 105.8 . 1_555 1_555 no C(16) C(15) C(22) 127.9(5) . 1_555 1_555 yes C(16) C(15) H(9) 109.2 . 1_555 1_555 no C(22) C(15) H(9) 120.8 . 1_555 1_555 no C(15) C(16) C(17) 115.6(4) . 1_555 1_555 yes C(15) C(16) H(10) 106.5 . 1_555 1_555 no C(15) C(16) H(11) 125.7 . 1_555 1_555 no C(17) C(16) H(10) 106.9 . 1_555 1_555 no C(17) C(16) H(11) 118.5 . 1_555 1_555 no H(10) C(16) H(11) 53.0 . 1_555 1_555 no C(16) C(17) C(18) 115.4(4) . 1_555 1_555 yes C(16) C(17) H(12) 90.4 . 1_555 1_555 no C(16) C(17) H(13) 122.0 . 1_555 1_555 no C(18) C(17) H(12) 107.9 . 1_555 1_555 no C(18) C(17) H(13) 119.7 . 1_555 1_555 no H(12) C(17) H(13) 89.1 . 1_555 1_555 no Rh(1) C(18) C(17) 112.6(3) . 1_555 1_555 yes Rh(1) C(18) C(19) 71.2(3) . 1_555 1_555 yes Rh(1) C(18) H(14) 106.7 . 1_555 1_555 no C(17) C(18) C(19) 125.3(5) . 1_555 1_555 yes C(17) C(18) H(14) 113.8 . 1_555 1_555 no C(19) C(18) H(14) 116.8 . 1_555 1_555 no Rh(1) C(19) C(18) 70.8(3) . 1_555 1_555 yes Rh(1) C(19) C(20) 109.0(3) . 1_555 1_555 yes Rh(1) C(19) H(15) 106.2 . 1_555 1_555 no C(18) C(19) C(20) 125.8(6) . 1_555 1_555 yes C(18) C(19) H(15) 119.9 . 1_555 1_555 no C(20) C(19) H(15) 112.1 . 1_555 1_555 no C(19) C(20) C(21) 117.8(4) . 1_555 1_555 yes C(19) C(20) H(16) 117.9 . 1_555 1_555 no C(19) C(20) H(17) 105.3 . 1_555 1_555 no C(21) C(20) H(16) 102.0 . 1_555 1_555 no C(21) C(20) H(17) 130.8 . 1_555 1_555 no H(16) C(20) H(17) 75.6 . 1_555 1_555 no C(20) C(21) C(22) 115.6(5) . 1_555 1_555 yes C(20) C(21) H(18) 110.5 . 1_555 1_555 no C(20) C(21) H(19) 103.2 . 1_555 1_555 no C(22) C(21) H(18) 112.9 . 1_555 1_555 no C(22) C(21) H(19) 111.0 . 1_555 1_555 no H(18) C(21) H(19) 102.4 . 1_555 1_555 no Rh(1) C(22) C(15) 70.9(3) . 1_555 1_555 yes Rh(1) C(22) C(21) 111.8(4) . 1_555 1_555 yes Rh(1) C(22) H(20) 101.3 . 1_555 1_555 no C(15) C(22) C(21) 124.0(5) . 1_555 1_555 yes C(15) C(22) H(20) 116.8 . 1_555 1_555 no C(21) C(22) H(20) 117.1 . 1_555 1_555 no O(1) C(24) C(23) 127(2) . 1_555 1_555 yes O(1) C(24) C(25) 110(2) . 1_555 1_555 yes C(23) C(24) C(25) 116(1) . 1_555 1_555 yes F(1) B(1) F(2) 126(1) . 1_555 1_555 yes F(1) B(1) F(3) 104.2(7) . 1_555 1_555 yes F(1) B(1) F(4) 105.2(7) . 1_555 1_555 yes F(2) B(1) F(3) 99.6(8) . 1_555 1_555 yes F(2) B(1) F(4) 106.6(8) . 1_555 1_555 yes F(3) B(1) F(4) 114(1) . 1_555 1_555 yes N(1) Rh(1) N(2) 86.4(2) . 1_555 1_555 yes N(1) Rh(1) C(15) 91.9(2) . 1_555 1_555 yes N(1) Rh(1) C(18) 164.2(1) . 1_555 1_555 yes N(1) Rh(1) C(22) 91.0(2) . 1_555 1_555 yes N(1) Rh(1) C(19) 157.8(2) . 1_555 1_555 yes N(2) Rh(1) C(15) 166.3(2) . 1_555 1_555 yes N(2) Rh(1) C(18) 95.8(2) . 1_555 1_555 yes N(2) Rh(1) C(22) 156.0(2) . 1_555 1_555 yes N(2) Rh(1) C(19) 91.5(2) . 1_555 1_555 yes C(15) Rh(1) C(18) 82.2(2) . 1_555 1_555 yes C(15) Rh(1) C(22) 37.6(2) . 1_555 1_555 yes C(15) Rh(1) C(19) 95.1(2) . 1_555 1_555 yes C(18) Rh(1) C(22) 93.1(2) . 1_555 1_555 yes C(18) Rh(1) C(19) 38.0(2) . 1_555 1_555 yes C(22) Rh(1) C(19) 81.9(2) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(12) 3.23(1) . 1_554 ? F(1) C(13) 3.355(9) . 1_554 ? F(1) C(2) 3.394(10) . 4_554 ? F(1) C(3) 3.398(8) . 3_666 ? F(2) C(21) 3.23(1) . 3_656 ? F(2) C(11) 3.381(9) . 2_646 ? F(2) C(20) 3.38(1) . 3_656 ? F(2) C(22) 3.44(1) . 3_656 ? F(3) C(12) 3.40(1) . 2_646 ? F(3) C(1) 3.490(10) . 3_656 ? F(3) C(23) 3.54(4) . 2_645 ? F(3) C(2) 3.58(1) . 4_554 ? F(4) C(14) 3.35(1) . 3_656 ? F(4) C(13) 3.51(1) . 1_554 ? O(1) C(6) 3.41(2) . 2_646 ? O(1) C(5) 3.53(2) . 2_646 ? O(1) C(4) 3.58(2) . 2_646 ? C(18) C(18) 3.333(8) . 3_557 ? #===END #------------------------------------------------------------------------------ data_rh-4bpbd-bf4.cif #(2a) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28 H32 B F4 N2 O2 Rh ' _chemical_formula_moiety '?' _chemical_formula_weight 618.28 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z -x,-y,-z x,1/2-y,z _cell_length_a 9.162(4) _cell_length_b 18.442(3) _cell_length_c 9.573(7) _cell_angle_alpha 90 _cell_angle_beta 108.79(5) _cell_angle_gamma 90 _cell_volume 1531(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.1 _cell_measurement_theta_max 13.6 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3838 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 5.25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 2457 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1373 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3624 _refine_ls_number_parameters 196 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.58 _refine_diff_density_min -0.77 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.006(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rh' 'Rh' -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh(1) Rh 0.25269(5) 0.2500 0.95038(6) 0.0454(1) Uani 1.00 d S . . F(1) F 0.622(4) 0.2500 0.424(3) 0.24(2) Uani 0.32 d SP . . F(2) F 0.407(1) 0.2500 0.3317(9) 0.184(5) Uani 0.90 d SP . . F(3) F 0.336(1) 0.2500 0.521(1) 0.138(5) Uani 0.66 d SP . . F(4) F 0.551(2) 0.2500 0.587(2) 0.23(2) Uani 0.65 d SP . . F(5) F 0.524(2) 0.183(1) 0.488(3) 0.27(1) Uani 0.72 d P . . O(1) O 0.1956(9) 0.0294(4) 0.6366(8) 0.173(3) Uani 1.00 d . . . N(1) N 0.4237(4) 0.3286(2) 0.9646(4) 0.050(1) Uani 1.00 d . . . C(1) C 0.5076(6) 0.3584(3) 1.0915(6) 0.069(2) Uani 1.00 d . . . C(2) C 0.6318(6) 0.4032(3) 1.1034(6) 0.074(2) Uani 1.00 d . . . C(3) C 0.6736(5) 0.4173(2) 0.9801(6) 0.054(1) Uani 1.00 d . . . C(4) C 0.5851(6) 0.3871(3) 0.8480(6) 0.066(2) Uani 1.00 d . . . C(5) C 0.4620(5) 0.3436(3) 0.8440(5) 0.063(1) Uani 1.00 d . . . C(6) C 0.8111(5) 0.4571(3) 0.9887(6) 0.063(1) Uani 1.00 d . . . C(7) C 0.9311(5) 0.4844(2) 0.9962(6) 0.062(1) Uani 1.00 d . . . C(8) C 0.1071(6) 0.3254(3) 1.0087(8) 0.075(2) Uani 1.00 d . . . C(9) C 0.0125(8) 0.2879(3) 1.0910(9) 0.119(3) Uani 1.00 d . . . C(10) C 0.0735(5) 0.1741(3) 0.8589(8) 0.077(2) Uani 1.00 d . . . C(11) C -0.0633(7) 0.2117(4) 0.7477(10) 0.140(3) Uani 1.00 d . . . C(12) C 0.101(2) 0.1042(8) 0.433(2) 0.228(7) Uani 1.00 d . . . C(13) C 0.191(1) 0.0421(8) 0.512(1) 0.167(5) Uani 1.00 d . . . C(14) C 0.258(2) 0.001(1) 0.431(2) 0.31(1) Uani 1.00 d . . . B(1) B 0.467(3) 0.2500 0.466(2) 0.136(9) Uani 1.00 d S . . H(1) H 0.4822 0.3473 1.1796 0.0829 Uiso 1.00 calc . . . H(2) H 0.6893 0.4251 1.1975 0.0883 Uiso 1.00 calc . . . H(3) H 0.6093 0.3966 0.7582 0.0802 Uiso 1.00 calc . . . H(4) H 0.4006 0.3230 0.7494 0.0759 Uiso 1.00 calc . . . H(5) H 0.1618 0.3687 1.0585 0.0889 Uiso 1.00 calc . . . H(6) H 0.0497 0.3042 1.1939 0.1483 Uiso 1.00 calc . . . H(7) H -0.0915 0.3042 1.0510 0.1483 Uiso 1.00 calc . . . H(8) H 0.1081 0.1307 0.8226 0.0916 Uiso 1.00 calc . . . H(9) H -0.0703 0.1946 0.6508 0.1621 Uiso 1.00 calc . . . H(10) H -0.1562 0.1946 0.7665 0.1621 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0314(2) 0.0350(2) 0.0719(4) 0.0000 0.0197(2) 0.0000 F(1) 0.12(3) 0.50(9) 0.10(2) 0.0000 0.03(1) 0.0000 F(2) 0.141(8) 0.33(2) 0.074(7) 0.0000 0.019(5) 0.0000 F(3) 0.126(10) 0.20(1) 0.101(7) 0.0000 0.060(6) 0.0000 F(4) 0.15(2) 0.43(7) 0.09(1) 0.0000 0.017(9) 0.0000 F(5) 0.38(2) 0.19(2) 0.28(3) 0.09(1) 0.15(2) 0.04(1) O(1) 0.234(8) 0.137(5) 0.132(5) 0.024(6) 0.039(5) 0.009(5) N(1) 0.041(2) 0.046(2) 0.068(2) -0.006(2) 0.024(2) 0.001(2) C(1) 0.064(3) 0.086(4) 0.065(3) -0.029(3) 0.033(3) -0.018(3) C(2) 0.059(3) 0.090(4) 0.076(4) -0.030(3) 0.028(3) -0.026(3) C(3) 0.040(2) 0.042(2) 0.083(3) -0.005(2) 0.024(2) -0.001(2) C(4) 0.060(3) 0.070(3) 0.075(3) -0.012(3) 0.029(3) 0.011(3) C(5) 0.050(3) 0.074(3) 0.065(3) -0.018(2) 0.018(2) -0.004(3) C(6) 0.049(2) 0.045(3) 0.097(4) -0.005(2) 0.028(2) -0.001(2) C(7) 0.048(2) 0.042(2) 0.103(4) -0.005(2) 0.031(3) 0.001(2) C(8) 0.068(3) 0.041(2) 0.138(6) 0.009(2) 0.062(4) -0.001(3) C(9) 0.132(6) 0.077(4) 0.203(8) -0.005(4) 0.129(6) -0.015(5) C(10) 0.046(3) 0.055(3) 0.129(5) -0.019(2) 0.026(3) -0.029(3) C(11) 0.070(4) 0.129(6) 0.171(7) 0.010(4) -0.030(4) -0.061(5) C(12) 0.26(2) 0.18(1) 0.18(1) -0.02(1) -0.01(1) 0.07(1) C(13) 0.20(1) 0.21(1) 0.079(6) -0.07(1) 0.022(7) -0.007(8) C(14) 0.31(2) 0.46(3) 0.20(1) 0.08(2) 0.13(1) -0.11(2) B(1) 0.15(2) 0.14(2) 0.09(2) 0.0000 -0.02(1) 0.0000 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) N(1) 2.107(3) . . yes Rh(1) N(1) 2.107(3) . 4_555 yes Rh(1) C(8) 2.123(5) . . yes Rh(1) C(8) 2.123(5) . 4_555 yes Rh(1) C(10) 2.120(5) . . yes Rh(1) C(10) 2.120(5) . 4_555 yes F(1) B(1) 1.59(4) . . yes F(2) B(1) 1.23(2) . . yes F(3) B(1) 1.45(2) . . yes F(4) F(5) 1.53(2) . . yes F(4) F(5) 1.53(2) . 4_555 yes F(4) B(1) 1.17(2) . . yes F(5) B(1) 1.34(2) . . yes O(1) C(13) 1.21(1) . . yes N(1) C(1) 1.329(6) . . yes N(1) C(5) 1.339(6) . . yes C(1) C(2) 1.382(6) . . yes C(1) H(1) 0.966 . . no C(2) C(3) 1.378(7) . . yes C(2) H(2) 0.972 . . no C(3) C(4) 1.381(7) . . yes C(3) C(6) 1.437(6) . . yes C(4) C(5) 1.374(6) . . yes C(4) H(3) 0.970 . . no C(5) H(4) 0.976 . . no C(6) C(7) 1.190(6) . . yes C(7) C(7) 1.369(8) . 3_767 yes C(8) C(9) 1.514(8) . . yes C(8) C(10) 1.366(8) . 4_555 yes C(8) H(5) 0.980 . . no C(9) C(9) 1.40(1) . 4_555 yes C(9) H(6) 0.980 . . no C(9) H(7) 0.954 . . no C(10) C(11) 1.525(9) . . yes C(10) H(8) 0.966 . . no C(11) C(11) 1.41(2) . 4_555 yes C(11) H(9) 0.962 . . no C(11) H(10) 0.977 . . no C(12) C(13) 1.47(2) . . yes C(13) C(14) 1.37(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Rh(1) N(1) 87.0(2) . 1_555 4_555 yes N(1) Rh(1) C(8) 92.8(2) . 1_555 1_555 yes N(1) Rh(1) C(8) 162.0(2) . 1_555 4_555 yes N(1) Rh(1) C(10) 160.4(2) . 1_555 1_555 yes N(1) Rh(1) C(10) 91.9(2) . 1_555 4_555 yes N(1) Rh(1) C(8) 162.0(2) . 4_555 1_555 yes N(1) Rh(1) C(8) 92.8(2) . 4_555 4_555 yes N(1) Rh(1) C(10) 91.9(2) . 4_555 1_555 yes N(1) Rh(1) C(10) 160.4(2) . 4_555 4_555 yes C(8) Rh(1) C(8) 81.9(3) . 1_555 4_555 yes C(8) Rh(1) C(10) 94.1(2) . 1_555 1_555 yes C(8) Rh(1) C(10) 37.6(2) . 1_555 4_555 yes C(8) Rh(1) C(10) 37.6(2) . 4_555 1_555 yes C(8) Rh(1) C(10) 94.1(2) . 4_555 4_555 yes C(10) Rh(1) C(10) 82.6(3) . 1_555 4_555 yes F(5) F(4) F(5) 108(1) . 1_555 4_555 yes F(5) F(4) B(1) 57.5(9) . 1_555 1_555 yes F(5) F(4) B(1) 57.5(9) . 4_555 1_555 yes F(4) F(5) B(1) 47(1) . 1_555 1_555 yes Rh(1) N(1) C(1) 122.8(3) . 1_555 1_555 yes Rh(1) N(1) C(5) 118.8(3) . 1_555 1_555 yes C(1) N(1) C(5) 117.9(4) . 1_555 1_555 yes N(1) C(1) C(2) 122.8(5) . 1_555 1_555 yes N(1) C(1) H(1) 118.7 . 1_555 1_555 no C(2) C(1) H(1) 118.5 . 1_555 1_555 no C(1) C(2) C(3) 119.4(5) . 1_555 1_555 yes C(1) C(2) H(2) 120.7 . 1_555 1_555 no C(3) C(2) H(2) 119.9 . 1_555 1_555 no C(2) C(3) C(4) 117.7(4) . 1_555 1_555 yes C(2) C(3) C(6) 121.8(5) . 1_555 1_555 yes C(4) C(3) C(6) 120.2(4) . 1_555 1_555 yes C(3) C(4) C(5) 119.7(4) . 1_555 1_555 yes C(3) C(4) H(3) 120.2 . 1_555 1_555 no C(5) C(4) H(3) 120.1 . 1_555 1_555 no N(1) C(5) C(4) 122.5(5) . 1_555 1_555 yes N(1) C(5) H(4) 119.2 . 1_555 1_555 no C(4) C(5) H(4) 118.3 . 1_555 1_555 no C(3) C(6) C(7) 174.2(5) . 1_555 1_555 yes C(6) C(7) C(7) 179.6(8) . 1_555 3_767 yes Rh(1) C(8) C(9) 110.6(4) . 1_555 1_555 yes Rh(1) C(8) C(10) 71.1(3) . 1_555 4_555 yes Rh(1) C(8) H(5) 113.3 . 1_555 1_555 no C(9) C(8) C(10) 125.2(6) . 1_555 4_555 yes C(9) C(8) H(5) 114.1 . 1_555 1_555 no C(10) C(8) H(5) 114.3 . 4_555 1_555 no C(8) C(9) C(9) 117.2(3) . 1_555 4_555 yes C(8) C(9) H(6) 108.1 . 1_555 1_555 no C(8) C(9) H(7) 108.2 . 1_555 1_555 no C(9) C(9) H(6) 107.9 . 4_555 1_555 no C(9) C(9) H(7) 108.4 . 4_555 1_555 no H(6) C(9) H(7) 106.6 . 1_555 1_555 no Rh(1) C(10) C(8) 71.3(3) . 1_555 4_555 yes Rh(1) C(10) C(11) 110.0(4) . 1_555 1_555 yes Rh(1) C(10) H(8) 113.3 . 1_555 1_555 no C(8) C(10) C(11) 125.9(6) . 4_555 1_555 yes C(8) C(10) H(8) 113.2 . 4_555 1_555 no C(11) C(10) H(8) 114.6 . 1_555 1_555 no C(10) C(11) C(11) 117.0(3) . 1_555 4_555 yes C(10) C(11) H(9) 108.0 . 1_555 1_555 no C(10) C(11) H(10) 107.0 . 1_555 1_555 no C(11) C(11) H(9) 109.2 . 4_555 1_555 no C(11) C(11) H(10) 108.9 . 4_555 1_555 no H(9) C(11) H(10) 106.3 . 1_555 1_555 no O(1) C(13) C(12) 119(1) . 1_555 1_555 yes O(1) C(13) C(14) 124(1) . 1_555 1_555 yes C(12) C(13) C(14) 115(1) . 1_555 1_555 yes F(1) B(1) F(2) 82(1) . 1_555 1_555 yes F(1) B(1) F(3) 174(1) . 1_555 1_555 yes F(1) B(1) F(4) 84(1) . 1_555 1_555 yes F(1) B(1) F(5) 72(1) . 1_555 1_555 yes F(1) B(1) F(5) 72(1) . 1_555 4_555 yes F(2) B(1) F(3) 103(1) . 1_555 1_555 yes F(2) B(1) F(4) 166(2) . 1_555 1_555 yes F(2) B(1) F(5) 100(1) . 1_555 1_555 yes F(2) B(1) F(5) 100(1) . 1_555 4_555 yes F(3) B(1) F(4) 90(1) . 1_555 1_555 yes F(3) B(1) F(5) 105(1) . 1_555 1_555 yes F(3) B(1) F(5) 105(1) . 1_555 4_555 yes F(4) B(1) F(5) 75(1) . 1_555 1_555 yes F(4) B(1) F(5) 75(1) . 1_555 4_555 yes F(5) B(1) F(5) 136(2) . 1_555 4_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Rh(1) F(2) 3.464(8) . 1_556 ? F(1) C(11) 3.56(3) . 1_655 ? F(1) C(11) 3.56(3) . 4_655 ? F(2) C(1) 3.392(8) . 1_554 ? F(2) C(1) 3.392(8) . 4_554 ? F(3) C(12) 3.38(1) . . ? F(3) C(12) 3.38(1) . 4_555 ? F(3) C(5) 3.405(10) . . ? F(3) C(5) 3.405(10) . 4_555 ? F(4) C(5) 3.31(2) . . ? F(4) C(5) 3.31(2) . 4_555 ? F(4) C(11) 3.44(2) . 1_655 ? F(4) C(11) 3.44(2) . 4_655 ? F(4) C(4) 3.49(1) . . ? F(4) C(4) 3.49(1) . 4_555 ? F(5) C(4) 3.55(2) . 4_555 ? O(1) C(2) 3.401(9) . 2_647 ? O(1) C(5) 3.502(9) . 4_555 ? O(1) C(12) 3.57(1) . 3_556 ? C(6) C(9) 3.598(9) . 1_655 ? C(6) C(8) 3.599(7) . 1_655 ? C(7) C(8) 3.329(6) . 1_655 ? C(7) C(8) 3.524(7) . 3_667 ? #===END #------------------------------------------------------------------------------ data_rh-4bpbd-pf6.cif #(2b) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28 H32 F6 N2 O2 P Rh ' _chemical_formula_moiety '?' _chemical_formula_weight 676.44 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z -x,-y,-z x,1/2-y,z _cell_length_a 9.347(2) _cell_length_b 18.114(3) _cell_length_c 9.917(3) _cell_angle_alpha 90 _cell_angle_beta 108.53(2) _cell_angle_gamma 90 _cell_volume 1592.1(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 12.1 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.996 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3989 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.52 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 28.50 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 2497 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1686 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3763 _refine_ls_number_parameters 190 _refine_ls_goodness_of_fit_ref 1.390 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.91 _refine_diff_density_min -1.07 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rh' 'Rh' -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh(1) Rh 0.26239(6) 0.2500 0.95407(7) 0.0417(2) Uani 1.00 d S . . P(1) P 0.4923(3) 0.2500 1.4712(3) 0.0830(10) Uani 1.00 d S . . F(1) F 0.497(2) 0.1704(5) 1.482(2) 0.297(7) Uani 1.00 d . . . F(2) F 0.3526(8) 0.2500 1.5269(7) 0.122(3) Uani 1.00 d S . . F(3) F 0.5940(9) 0.2500 1.6233(8) 0.209(5) Uani 1.00 d S . . F(4) F 0.6278(9) 0.2500 1.4150(9) 0.194(5) Uani 1.00 d S . . F(5) F 0.3936(10) 0.2500 1.3255(8) 0.269(7) Uani 1.00 d S . . O(1) O 0.195(1) 0.0317(4) 0.6342(8) 0.158(3) Uani 1.00 d . . . N(1) N 0.4306(4) 0.1698(2) 0.9674(5) 0.047(1) Uani 1.00 d . . . C(1) C 0.4654(6) 0.1528(4) 0.8508(6) 0.066(2) Uani 1.00 d . . . C(2) C 0.5888(7) 0.1100(4) 0.8561(6) 0.066(2) Uani 1.00 d . . . C(3) C 0.6794(5) 0.0817(3) 0.9830(6) 0.051(2) Uani 1.00 d . . . C(4) C 0.6395(7) 0.0979(4) 1.1029(7) 0.074(2) Uani 1.00 d . . . C(5) C 0.5153(7) 0.1409(4) 1.0903(6) 0.067(2) Uani 1.00 d . . . C(6) C 0.8136(6) 0.0425(3) 0.9922(7) 0.058(2) Uani 1.00 d . . . C(7) C 0.9321(6) 0.0155(3) 0.9966(7) 0.058(2) Uani 1.00 d . . . C(8) C 0.0859(6) 0.1719(3) 0.8649(8) 0.070(2) Uani 1.00 d . . . C(9) C -0.0458(8) 0.2104(5) 0.760(1) 0.134(3) Uani 1.00 d . . . C(10) C 0.1200(7) 0.1733(3) 1.0101(8) 0.065(2) Uani 1.00 d . . . C(11) C 0.024(1) 0.2119(4) 1.085(1) 0.112(3) Uani 1.00 d . . . C(12) C 0.254(2) -0.005(1) 0.434(2) 0.26(1) Uani 1.00 d . . . C(13) C 0.186(1) 0.0414(8) 0.513(1) 0.135(5) Uani 1.00 d . . . C(14) C 0.092(2) 0.1025(8) 0.436(2) 0.190(6) Uani 1.00 d . . . H(1) H 0.3985 0.1711 0.7626 0.0802 Uiso 1.00 calc . . . H(2) H 0.6074 0.1010 0.7664 0.0799 Uiso 1.00 calc . . . H(3) H 0.6902 0.0756 1.1952 0.0928 Uiso 1.00 calc . . . H(4) H 0.4827 0.1519 1.1697 0.0864 Uiso 1.00 calc . . . H(5) H 0.1205 0.1278 0.8318 0.0790 Uiso 1.00 calc . . . H(6) H -0.0441 0.1929 0.6665 0.1480 Uiso 1.00 calc . . . H(7) H -0.1332 0.1929 0.7744 0.1480 Uiso 1.00 calc . . . H(8) H 0.1700 0.1301 1.0569 0.0778 Uiso 1.00 calc . . . H(9) H 0.0594 0.1930 1.1832 0.1494 Uiso 1.00 calc . . . H(10) H -0.0769 0.1930 1.0443 0.1494 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0235(3) 0.0372(3) 0.0646(4) 0.0000 0.0142(2) 0.0000 P(1) 0.062(2) 0.131(3) 0.053(2) 0.0000 0.015(1) 0.0000 F(1) 0.38(2) 0.138(7) 0.48(2) 0.035(9) 0.28(2) 0.009(9) F(2) 0.073(4) 0.207(8) 0.089(4) 0.0000 0.033(3) 0.0000 F(3) 0.077(5) 0.45(2) 0.086(5) 0.0000 0.009(4) 0.0000 F(4) 0.091(6) 0.39(2) 0.113(6) 0.0000 0.051(5) 0.0000 F(5) 0.094(6) 0.64(3) 0.060(5) 0.0000 0.013(4) 0.0000 O(1) 0.207(9) 0.152(7) 0.101(5) 0.010(7) 0.028(5) 0.004(5) N(1) 0.029(2) 0.048(2) 0.066(3) 0.009(2) 0.017(2) 0.002(2) C(1) 0.047(3) 0.090(5) 0.060(4) 0.027(3) 0.017(3) 0.004(3) C(2) 0.056(3) 0.084(4) 0.064(4) 0.022(3) 0.026(3) -0.006(3) C(3) 0.031(2) 0.043(3) 0.079(4) 0.007(2) 0.018(3) 0.001(3) C(4) 0.052(3) 0.100(5) 0.069(4) 0.034(4) 0.019(3) 0.014(4) C(5) 0.056(3) 0.088(5) 0.059(4) 0.029(3) 0.021(3) 0.011(3) C(6) 0.039(3) 0.045(3) 0.092(4) 0.008(2) 0.024(3) 0.004(3) C(7) 0.041(3) 0.038(3) 0.099(4) 0.007(2) 0.029(3) 0.001(3) C(8) 0.036(3) 0.045(3) 0.122(6) -0.013(2) 0.017(3) -0.024(4) C(9) 0.056(4) 0.130(8) 0.167(8) 0.009(4) -0.034(5) -0.061(6) C(10) 0.055(3) 0.040(3) 0.109(5) -0.011(3) 0.040(4) -0.003(3) C(11) 0.122(7) 0.077(5) 0.187(9) -0.005(5) 0.119(7) 0.000(5) C(12) 0.35(3) 0.24(2) 0.25(2) -0.01(2) 0.20(2) -0.08(1) C(13) 0.137(9) 0.17(1) 0.083(7) -0.062(9) 0.018(6) -0.006(7) C(14) 0.16(1) 0.17(1) 0.19(1) -0.03(1) -0.014(10) 0.08(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) N(1) 2.115(4) . . yes Rh(1) N(1) 2.115(4) . 4_555 yes Rh(1) C(8) 2.140(5) . . yes Rh(1) C(8) 2.140(5) . 4_555 yes Rh(1) C(10) 2.117(5) . . yes Rh(1) C(10) 2.117(5) . 4_555 yes P(1) F(1) 1.446(10) . . yes P(1) F(1) 1.446(10) . 4_555 yes P(1) F(2) 1.571(7) . . yes P(1) F(3) 1.506(8) . . yes P(1) F(4) 1.538(8) . . yes P(1) F(5) 1.446(8) . . yes O(1) C(13) 1.19(1) . . yes N(1) C(1) 1.332(7) . . yes N(1) C(5) 1.332(7) . . yes C(1) C(2) 1.377(7) . . yes C(1) H(1) 0.959 . . no C(2) C(3) 1.373(8) . . yes C(2) H(2) 0.973 . . no C(3) C(4) 1.386(8) . . yes C(3) C(6) 1.419(7) . . yes C(4) C(5) 1.370(8) . . yes C(4) H(3) 0.975 . . no C(5) H(4) 0.951 . . no C(6) C(7) 1.199(7) . . yes C(7) C(7) 1.370(10) . 3_757 yes C(8) C(9) 1.51(1) . . yes C(8) C(10) 1.373(9) . . yes C(8) H(5) 0.957 . . no C(9) C(9) 1.43(2) . 4_555 yes C(9) H(6) 0.983 . . no C(9) H(7) 0.930 . . no C(10) C(11) 1.504(9) . . yes C(10) H(8) 0.953 . . no C(11) C(11) 1.38(2) . 4_555 yes C(11) H(9) 0.985 . . no C(11) H(10) 0.966 . . no C(12) C(13) 1.43(2) . . yes C(13) C(14) 1.47(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Rh(1) N(1) 86.8(2) . 1_555 4_555 yes N(1) Rh(1) C(8) 91.8(2) . 1_555 1_555 yes N(1) Rh(1) C(8) 160.2(2) . 1_555 4_555 yes N(1) Rh(1) C(10) 92.9(2) . 1_555 1_555 yes N(1) Rh(1) C(10) 162.2(2) . 1_555 4_555 yes N(1) Rh(1) C(8) 160.2(2) . 4_555 1_555 yes N(1) Rh(1) C(8) 91.8(2) . 4_555 4_555 yes N(1) Rh(1) C(10) 162.2(2) . 4_555 1_555 yes N(1) Rh(1) C(10) 92.9(2) . 4_555 4_555 yes C(8) Rh(1) C(8) 82.8(3) . 1_555 4_555 yes C(8) Rh(1) C(10) 37.6(3) . 1_555 1_555 yes C(8) Rh(1) C(10) 94.4(2) . 1_555 4_555 yes C(8) Rh(1) C(10) 94.4(2) . 4_555 1_555 yes C(8) Rh(1) C(10) 37.6(3) . 4_555 4_555 yes C(10) Rh(1) C(10) 82.0(3) . 1_555 4_555 yes F(1) P(1) F(1) 172(1) . 1_555 4_555 yes F(1) P(1) F(2) 89.1(5) . 1_555 1_555 yes F(1) P(1) F(3) 86.2(7) . 1_555 1_555 yes F(1) P(1) F(4) 91.0(5) . 1_555 1_555 yes F(1) P(1) F(5) 93.8(7) . 1_555 1_555 yes F(1) P(1) F(2) 89.1(5) . 4_555 1_555 yes F(1) P(1) F(3) 86.2(7) . 4_555 1_555 yes F(1) P(1) F(4) 91.0(5) . 4_555 1_555 yes F(1) P(1) F(5) 93.8(7) . 4_555 1_555 yes F(2) P(1) F(3) 88.8(4) . 1_555 1_555 yes F(2) P(1) F(4) 179.4(4) . 1_555 1_555 yes F(2) P(1) F(5) 90.8(4) . 1_555 1_555 yes F(3) P(1) F(4) 91.9(5) . 1_555 1_555 yes F(3) P(1) F(5) 179.6(5) . 1_555 1_555 yes F(4) P(1) F(5) 88.6(5) . 1_555 1_555 yes Rh(1) N(1) C(1) 119.1(4) . 1_555 1_555 yes Rh(1) N(1) C(5) 122.7(4) . 1_555 1_555 yes C(1) N(1) C(5) 117.8(5) . 1_555 1_555 yes N(1) C(1) C(2) 121.9(5) . 1_555 1_555 yes N(1) C(1) H(1) 116.3 . 1_555 1_555 no C(2) C(1) H(1) 121.7 . 1_555 1_555 no C(1) C(2) C(3) 120.7(5) . 1_555 1_555 yes C(1) C(2) H(2) 116.8 . 1_555 1_555 no C(3) C(2) H(2) 122.5 . 1_555 1_555 no C(2) C(3) C(4) 116.8(5) . 1_555 1_555 yes C(2) C(3) C(6) 121.4(5) . 1_555 1_555 yes C(4) C(3) C(6) 121.6(5) . 1_555 1_555 yes C(3) C(4) C(5) 119.6(5) . 1_555 1_555 yes C(3) C(4) H(3) 122.3 . 1_555 1_555 no C(5) C(4) H(3) 117.8 . 1_555 1_555 no N(1) C(5) C(4) 123.1(5) . 1_555 1_555 yes N(1) C(5) H(4) 115.0 . 1_555 1_555 no C(4) C(5) H(4) 121.9 . 1_555 1_555 no C(3) C(6) C(7) 173.8(6) . 1_555 1_555 yes C(6) C(7) C(7) 179.3(9) . 1_555 3_757 yes Rh(1) C(8) C(9) 109.4(5) . 1_555 1_555 yes Rh(1) C(8) C(10) 70.3(3) . 1_555 1_555 yes Rh(1) C(8) H(5) 113.1 . 1_555 1_555 no C(9) C(8) C(10) 125.7(7) . 1_555 1_555 yes C(9) C(8) H(5) 116.1 . 1_555 1_555 no C(10) C(8) H(5) 112.6 . 1_555 1_555 no C(8) C(9) C(9) 117.6(4) . 1_555 4_555 yes C(8) C(9) H(6) 104.3 . 1_555 1_555 no C(8) C(9) H(7) 107.3 . 1_555 1_555 no C(9) C(9) H(6) 108.8 . 4_555 1_555 no C(9) C(9) H(7) 110.0 . 4_555 1_555 no H(6) C(9) H(7) 108.3 . 1_555 1_555 no Rh(1) C(10) C(8) 72.1(3) . 1_555 1_555 yes Rh(1) C(10) C(11) 110.3(4) . 1_555 1_555 yes Rh(1) C(10) H(8) 114.5 . 1_555 1_555 no C(8) C(10) C(11) 123.4(7) . 1_555 1_555 yes C(8) C(10) H(8) 114.1 . 1_555 1_555 no C(11) C(10) H(8) 114.7 . 1_555 1_555 no C(10) C(11) C(11) 117.7(3) . 1_555 4_555 yes C(10) C(11) H(9) 105.3 . 1_555 1_555 no C(10) C(11) H(10) 106.6 . 1_555 1_555 no C(11) C(11) H(9) 110.3 . 4_555 1_555 no C(11) C(11) H(10) 110.7 . 4_555 1_555 no H(9) C(11) H(10) 105.3 . 1_555 1_555 no O(1) C(13) C(12) 124(1) . 1_555 1_555 yes O(1) C(13) C(14) 118(1) . 1_555 1_555 yes C(12) C(13) C(14) 116(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Rh(1) F(5) 3.493(7) . . ? F(2) C(1) 3.518(8) . 1_556 ? F(2) C(1) 3.518(8) . 4_556 ? F(2) C(14) 3.53(1) . 1_556 ? F(2) C(14) 3.53(1) . 4_556 ? F(3) C(9) 3.28(1) . 1_656 ? F(3) C(9) 3.28(1) . 4_656 ? F(3) C(1) 3.370(10) . 1_556 ? F(3) C(1) 3.370(10) . 4_556 ? F(3) C(2) 3.440(9) . 1_556 ? F(3) C(2) 3.440(9) . 4_556 ? F(5) C(5) 3.511(9) . . ? F(5) C(5) 3.511(9) . 4_555 ? F(5) C(11) 3.58(1) . . ? F(5) C(11) 3.58(1) . 4_555 ? O(1) C(4) 3.48(1) . 3_657 ? O(1) C(1) 3.51(1) . . ? O(1) C(14) 3.53(2) . 3_556 ? C(7) C(10) 3.336(8) . 1_655 ? C(7) C(10) 3.452(8) . 3_657 ? #===END #------------------------------------------------------------------------------ data_rh-2bpe-bf4.cif #(3a) #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C23 H28 B F4 N2 O Rh ' _chemical_formula_moiety 'C23 H28 B F4 N2 O Rh ' _chemical_formula_weight 538.20 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/b 21/c 21/a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _cell_length_a 15.153(3) _cell_length_b 16.4660(5) _cell_length_c 19.698(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4914.9(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 5117 _cell_measurement_theta_min ? _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_reflns_number 5117 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max ? _diffrn_measured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 2203 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.1880 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 5092 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 1.292 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0050 _refine_diff_density_max 1.25 _refine_diff_density_min -1.04 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rh' 'Rh' -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh(1) Rh 0.81700(5) 0.11725(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(1) N 0.7248(6) 0.2021(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . N(2) N 0.2621(6) 0.5258(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(1) C 0.6681(8) 0.2813(5) 0.2555(4) 0.058(3) Uani 1.00 d . . . C(2) C 0.7292(8) 0.2296(5) 0.2279(4) 0.057(3) Uani 1.00 d . . . C(3) C 0.6554(7) 0.2262(6) 0.1261(4) 0.061(3) Uani 1.00 d . . . C(4) C 0.5912(9) 0.2753(6) 0.1517(4) 0.070(4) Uani 1.00 d . . . C(5) C 0.5964(8) 0.3039(5) 0.2181(4) 0.053(3) Uani 1.00 d . . . C(6) C 0.5283(8) 0.3563(5) 0.2504(4) 0.058(3) Uani 1.00 d . . . C(7) C 0.4496(8) 0.3725(5) 0.2284(4) 0.057(3) Uani 1.00 d . . . C(8) C 0.3856(7) 0.4243(4) 0.2639(4) 0.050(3) Uani 1.00 d . . . C(9) C 0.3112(9) 0.4529(5) 0.2318(4) 0.057(3) Uani 1.00 d . . . C(10) C 0.2526(7) 0.5029(5) 0.2649(4) 0.051(3) Uani 1.00 d . . . C(11) C 0.3317(8) 0.4979(5) 0.3610(4) 0.064(3) Uani 1.00 d . . . C(12) C 0.3952(8) 0.4464(5) 0.3319(4) 0.067(4) Uani 1.00 d . . . C(13) C 0.8763(8) 0.2062(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14) C 0.9154(8) 0.2078(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17) C 0.9288(7) 0.0377(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18) C 0.8791(7) 0.0359(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . N(2*) N 0.7379(6) 0.0258(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . Rh(1*) Rh 0.18300(5) 0.61725(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . C(10*) C 0.7474(7) 0.0029(5) 0.2351(4) 0.051(3) Uani 1.00 d . . . C(11*) C 0.6683(8) -0.0021(5) 0.1390(4) 0.064(3) Uani 1.00 d . . . N(1*) N 0.2752(6) 0.7021(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . C(13*) C 0.1237(8) 0.7062(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14*) C 0.0846(8) 0.7078(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17*) C 0.0712(7) 0.5377(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18*) C 0.1209(7) 0.5359(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . C(9*) C 0.6888(9) -0.0471(5) 0.2682(4) 0.057(3) Uani 1.00 d . . . C(12*) C 0.6048(8) -0.0536(5) 0.1681(4) 0.067(4) Uani 1.00 d . . . C(2*) C 0.2708(8) 0.7296(5) 0.2721(4) 0.057(3) Uani 1.00 d . . . C(3*) C 0.3446(7) 0.7262(6) 0.3739(4) 0.061(3) Uani 1.00 d . . . C(8*) C 0.6144(7) -0.0757(4) 0.2361(4) 0.050(3) Uani 1.00 d . . . C(1*) C 0.3319(8) 0.7813(5) 0.2445(4) 0.058(3) Uani 1.00 d . . . C(4*) C 0.4088(9) 0.7753(6) 0.3483(4) 0.070(4) Uani 1.00 d . . . C(7*) C 0.5504(8) -0.1275(5) 0.2716(4) 0.057(3) Uani 1.00 d . . . C(5*) C 0.4036(8) 0.8039(5) 0.2819(4) 0.053(3) Uani 1.00 d . . . C(6*) C 0.4717(8) -0.1437(5) 0.2496(4) 0.058(3) Uani 1.00 d . . . C(6*) C 0.4717(8) 0.8563(5) 0.2496(4) 0.058(3) Uani 1.00 d . . . C(5*) C 0.4036(8) -0.1961(5) 0.2819(4) 0.053(3) Uani 1.00 d . . . C(7*) C 0.5504(8) 0.8725(5) 0.2716(4) 0.057(3) Uani 1.00 d . . . C(1*) C 0.3319(8) -0.2187(5) 0.2445(4) 0.058(3) Uani 1.00 d . . . C(4*) C 0.4088(9) -0.2247(6) 0.3483(4) 0.070(4) Uani 1.00 d . . . C(8*) C 0.6144(7) 0.9243(4) 0.2361(4) 0.050(3) Uani 1.00 d . . . C(2*) C 0.2708(8) -0.2704(5) 0.2721(4) 0.057(3) Uani 1.00 d . . . C(3*) C 0.3446(7) -0.2738(6) 0.3739(4) 0.061(3) Uani 1.00 d . . . C(9*) C 0.6888(9) 0.9529(5) 0.2682(4) 0.057(3) Uani 1.00 d . . . C(12*) C 0.6048(8) 0.9464(5) 0.1681(4) 0.067(4) Uani 1.00 d . . . N(1*) N 0.2752(6) -0.2979(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . C(10*) C 0.7474(7) 1.0029(5) 0.2351(4) 0.051(3) Uani 1.00 d . . . C(11*) C 0.6683(8) 0.9979(5) 0.1390(4) 0.064(3) Uani 1.00 d . . . Rh(1*) Rh 0.18300(5) -0.38275(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . N(2*) N 0.7379(6) 1.0258(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . N(2') N 0.2621(6) -0.4742(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(13*) C 0.1237(8) -0.2938(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14*) C 0.0846(8) -0.2922(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17*) C 0.0712(7) -0.4623(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18*) C 0.1209(7) -0.4641(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . Rh(1') Rh 0.81700(5) 1.11725(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(1') N 0.7248(6) 1.2021(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . C(13') C 0.8763(8) 1.2062(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14') C 0.9154(8) 1.2078(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17') C 0.9288(7) 1.0377(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18') C 0.8791(7) 1.0359(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . Rh(1*) Rh 1.81700(5) 0.11725(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(1*) N 1.7248(6) 0.2021(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . N(2*) N 1.2621(6) 0.5258(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(1*) C 1.6681(8) 0.2813(5) 0.2555(4) 0.058(3) Uani 1.00 d . . . C(2*) C 1.7292(8) 0.2296(5) 0.2279(4) 0.057(3) Uani 1.00 d . . . C(3*) C 1.6554(7) 0.2262(6) 0.1261(4) 0.061(3) Uani 1.00 d . . . C(4*) C 1.5912(9) 0.2753(6) 0.1517(4) 0.070(4) Uani 1.00 d . . . C(5*) C 1.5964(8) 0.3039(5) 0.2181(4) 0.053(3) Uani 1.00 d . . . C(6*) C 1.5283(8) 0.3563(5) 0.2504(4) 0.058(3) Uani 1.00 d . . . C(7*) C 1.4496(8) 0.3725(5) 0.2284(4) 0.057(3) Uani 1.00 d . . . C(8*) C 1.3856(7) 0.4243(4) 0.2639(4) 0.050(3) Uani 1.00 d . . . C(9*) C 1.3112(9) 0.4529(5) 0.2318(4) 0.057(3) Uani 1.00 d . . . C(10*) C 1.2526(7) 0.5029(5) 0.2649(4) 0.051(3) Uani 1.00 d . . . C(11*) C 1.3317(8) 0.4979(5) 0.3610(4) 0.064(3) Uani 1.00 d . . . C(12*) C 1.3952(8) 0.4464(5) 0.3319(4) 0.067(4) Uani 1.00 d . . . C(13*) C 1.8763(8) 0.2062(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14*) C 1.9154(8) 0.2078(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17*) C 1.9288(7) 0.0377(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18*) C 1.8791(7) 0.0359(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . N(2**) N 1.7379(6) 0.0258(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . Rh(1**) Rh 1.18300(5) 0.61725(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . C(10**) C 1.7474(7) 0.0029(5) 0.2351(4) 0.051(3) Uani 1.00 d . . . C(11**) C 1.6683(8) -0.0021(5) 0.1390(4) 0.064(3) Uani 1.00 d . . . N(1**) N 1.2752(6) 0.7021(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . C(13**) C 1.1237(8) 0.7062(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14**) C 1.0846(8) 0.7078(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17**) C 1.0712(7) 0.5377(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18**) C 1.1209(7) 0.5359(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . C(9**) C 1.6888(9) -0.0471(5) 0.2682(4) 0.057(3) Uani 1.00 d . . . C(12**) C 1.6048(8) -0.0536(5) 0.1681(4) 0.067(4) Uani 1.00 d . . . C(2**) C 1.2708(8) 0.7296(5) 0.2721(4) 0.057(3) Uani 1.00 d . . . C(3**) C 1.3446(7) 0.7262(6) 0.3739(4) 0.061(3) Uani 1.00 d . . . C(8**) C 1.6144(7) -0.0757(4) 0.2361(4) 0.050(3) Uani 1.00 d . . . C(1**) C 1.3319(8) 0.7813(5) 0.2445(4) 0.058(3) Uani 1.00 d . . . C(4**) C 1.4088(9) 0.7753(6) 0.3483(4) 0.070(4) Uani 1.00 d . . . C(7**) C 1.5504(8) -0.1275(5) 0.2716(4) 0.057(3) Uani 1.00 d . . . C(5**) C 1.4036(8) 0.8039(5) 0.2819(4) 0.053(3) Uani 1.00 d . . . C(6**) C 1.4717(8) -0.1437(5) 0.2496(4) 0.058(3) Uani 1.00 d . . . C(6**) C 1.4717(8) 0.8563(5) 0.2496(4) 0.058(3) Uani 1.00 d . . . C(5**) C 1.4036(8) -0.1961(5) 0.2819(4) 0.053(3) Uani 1.00 d . . . C(7**) C 1.5504(8) 0.8725(5) 0.2716(4) 0.057(3) Uani 1.00 d . . . C(1**) C 1.3319(8) -0.2187(5) 0.2445(4) 0.058(3) Uani 1.00 d . . . C(4**) C 1.4088(9) -0.2247(6) 0.3483(4) 0.070(4) Uani 1.00 d . . . C(8**) C 1.6144(7) 0.9243(4) 0.2361(4) 0.050(3) Uani 1.00 d . . . C(2**) C 1.2708(8) -0.2704(5) 0.2721(4) 0.057(3) Uani 1.00 d . . . C(3**) C 1.3446(7) -0.2738(6) 0.3739(4) 0.061(3) Uani 1.00 d . . . C(9**) C 1.6888(9) 0.9529(5) 0.2682(4) 0.057(3) Uani 1.00 d . . . C(12**) C 1.6048(8) 0.9464(5) 0.1681(4) 0.067(4) Uani 1.00 d . . . N(1**) N 1.2752(6) -0.2979(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . C(10**) C 1.7474(7) 1.0029(5) 0.2351(4) 0.051(3) Uani 1.00 d . . . C(11**) C 1.6683(8) 0.9979(5) 0.1390(4) 0.064(3) Uani 1.00 d . . . Rh(1**) Rh 1.18300(5) -0.38275(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . N(2**) N 1.7379(6) 1.0258(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . N(2'*) N 1.2621(6) -0.4742(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(13**) C 1.1237(8) -0.2938(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14**) C 1.0846(8) -0.2922(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17**) C 1.0712(7) -0.4623(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18**) C 1.1209(7) -0.4641(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . Rh(1'*) Rh 1.81700(5) 1.11725(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(1'*) N 1.7248(6) 1.2021(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . C(13'*) C 1.8763(8) 1.2062(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14'*) C 1.9154(8) 1.2078(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17'*) C 1.9288(7) 1.0377(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18'*) C 1.8791(7) 1.0359(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . Rh(1*) Rh -0.31700(5) 0.61725(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(1*) N -0.2248(6) 0.7021(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . N(2*) N 0.2379(6) 1.0258(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(1*) C -0.1681(8) 0.7813(5) 0.2555(4) 0.058(3) Uani 1.00 d . . . C(2*) C -0.2292(8) 0.7296(5) 0.2279(4) 0.057(3) Uani 1.00 d . . . C(3*) C -0.1554(7) 0.7262(6) 0.1261(4) 0.061(3) Uani 1.00 d . . . C(4*) C -0.0912(9) 0.7753(6) 0.1517(4) 0.070(4) Uani 1.00 d . . . C(5*) C -0.0964(8) 0.8039(5) 0.2181(4) 0.053(3) Uani 1.00 d . . . C(6*) C -0.0283(8) 0.8563(5) 0.2504(4) 0.058(3) Uani 1.00 d . . . C(7*) C 0.0504(8) 0.8725(5) 0.2284(4) 0.057(3) Uani 1.00 d . . . C(8*) C 0.1144(7) 0.9243(4) 0.2639(4) 0.050(3) Uani 1.00 d . . . C(9*) C 0.1888(9) 0.9529(5) 0.2318(4) 0.057(3) Uani 1.00 d . . . C(10*) C 0.2474(7) 1.0029(5) 0.2649(4) 0.051(3) Uani 1.00 d . . . C(11*) C 0.1683(8) 0.9979(5) 0.3610(4) 0.064(3) Uani 1.00 d . . . C(12*) C 0.1048(8) 0.9464(5) 0.3319(4) 0.067(4) Uani 1.00 d . . . C(13*) C -0.3763(8) 0.7062(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14*) C -0.4154(8) 0.7078(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17*) C -0.4288(7) 0.5377(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18*) C -0.3791(7) 0.5359(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . N(2**) N -0.2379(6) 0.5258(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . Rh(1**) Rh 0.31700(5) 1.11725(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . C(10**) C -0.2474(7) 0.5029(5) 0.2351(4) 0.051(3) Uani 1.00 d . . . C(11**) C -0.1683(8) 0.4979(5) 0.1390(4) 0.064(3) Uani 1.00 d . . . N(1**) N 0.2248(6) 1.2021(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . C(13**) C 0.3763(8) 1.2062(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14**) C 0.4154(8) 1.2078(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17**) C 0.4288(7) 1.0377(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18**) C 0.3791(7) 1.0359(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . C(9**) C -0.1888(9) 0.4529(5) 0.2682(4) 0.057(3) Uani 1.00 d . . . C(12**) C -0.1048(8) 0.4464(5) 0.1681(4) 0.067(4) Uani 1.00 d . . . C(8**) C -0.1144(7) 0.4243(4) 0.2361(4) 0.050(3) Uani 1.00 d . . . C(7**) C -0.0504(8) 0.3725(5) 0.2716(4) 0.057(3) Uani 1.00 d . . . C(6**) C 0.0283(8) 0.3563(5) 0.2496(4) 0.058(3) Uani 1.00 d . . . C(5**) C 0.0964(8) 0.3039(5) 0.2819(4) 0.053(3) Uani 1.00 d . . . C(1**) C 0.1681(8) 0.2813(5) 0.2445(4) 0.058(3) Uani 1.00 d . . . C(4**) C 0.0912(9) 0.2753(6) 0.3483(4) 0.070(4) Uani 1.00 d . . . C(2**) C 0.2292(8) 0.2296(5) 0.2721(4) 0.057(3) Uani 1.00 d . . . C(3**) C 0.1554(7) 0.2262(6) 0.3739(4) 0.061(3) Uani 1.00 d . . . N(1**) N 0.2248(6) 0.2021(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . Rh(1**) Rh 0.31700(5) 0.11725(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . N(2'*) N 0.2379(6) 0.0258(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(13**) C 0.3763(8) 0.2062(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14**) C 0.4154(8) 0.2078(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17**) C 0.4288(7) 0.0377(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18**) C 0.3791(7) 0.0359(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . C(10'*) C 0.2474(7) 0.0029(5) 0.2649(4) 0.051(3) Uani 1.00 d . . . C(11'*) C 0.1683(8) -0.0021(5) 0.3610(4) 0.064(3) Uani 1.00 d . . . C(9'*) C 0.1888(9) -0.0471(5) 0.2318(4) 0.057(3) Uani 1.00 d . . . C(12'*) C 0.1048(8) -0.0536(5) 0.3319(4) 0.067(4) Uani 1.00 d . . . C(8'*) C 0.1144(7) -0.0757(4) 0.2639(4) 0.050(3) Uani 1.00 d . . . C(7'*) C 0.0504(8) -0.1275(5) 0.2284(4) 0.057(3) Uani 1.00 d . . . C(6'*) C -0.0283(8) -0.1437(5) 0.2504(4) 0.058(3) Uani 1.00 d . . . C(5'*) C -0.0964(8) -0.1961(5) 0.2181(4) 0.053(3) Uani 1.00 d . . . C(1'*) C -0.1681(8) -0.2187(5) 0.2555(4) 0.058(3) Uani 1.00 d . . . C(4'*) C -0.0912(9) -0.2247(6) 0.1517(4) 0.070(4) Uani 1.00 d . . . C(2'*) C -0.2292(8) -0.2704(5) 0.2279(4) 0.057(3) Uani 1.00 d . . . C(3'*) C -0.1554(7) -0.2738(6) 0.1261(4) 0.061(3) Uani 1.00 d . . . N(1'*) N -0.2248(6) -0.2979(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . Rh(1'*) Rh -0.31700(5) -0.38275(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(2**) N -0.2379(6) -0.4742(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . C(13'*) C -0.3763(8) -0.2938(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14'*) C -0.4154(8) -0.2922(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17'*) C -0.4288(7) -0.4623(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18'*) C -0.3791(7) -0.4641(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . Rh(1*) Rh 0.68300(5) 0.61725(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(1*) N 0.7752(6) 0.7021(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . N(2*) N 1.2379(6) 1.0258(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(1*) C 0.8319(8) 0.7813(5) 0.2555(4) 0.058(3) Uani 1.00 d . . . C(2*) C 0.7708(8) 0.7296(5) 0.2279(4) 0.057(3) Uani 1.00 d . . . C(3*) C 0.8446(7) 0.7262(6) 0.1261(4) 0.061(3) Uani 1.00 d . . . C(4*) C 0.9088(9) 0.7753(6) 0.1517(4) 0.070(4) Uani 1.00 d . . . C(5*) C 0.9036(8) 0.8039(5) 0.2181(4) 0.053(3) Uani 1.00 d . . . C(6*) C 0.9717(8) 0.8563(5) 0.2504(4) 0.058(3) Uani 1.00 d . . . C(7*) C 1.0504(8) 0.8725(5) 0.2284(4) 0.057(3) Uani 1.00 d . . . C(8*) C 1.1144(7) 0.9243(4) 0.2639(4) 0.050(3) Uani 1.00 d . . . C(9*) C 1.1888(9) 0.9529(5) 0.2318(4) 0.057(3) Uani 1.00 d . . . C(10*) C 1.2474(7) 1.0029(5) 0.2649(4) 0.051(3) Uani 1.00 d . . . C(11*) C 1.1683(8) 0.9979(5) 0.3610(4) 0.064(3) Uani 1.00 d . . . C(12*) C 1.1048(8) 0.9464(5) 0.3319(4) 0.067(4) Uani 1.00 d . . . C(13*) C 0.6237(8) 0.7062(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14*) C 0.5846(8) 0.7078(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17*) C 0.5712(7) 0.5377(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18*) C 0.6209(7) 0.5359(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . N(2**) N 0.7621(6) 0.5258(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . Rh(1**) Rh 1.31700(5) 1.11725(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . C(10**) C 0.7526(7) 0.5029(5) 0.2351(4) 0.051(3) Uani 1.00 d . . . C(11**) C 0.8317(8) 0.4979(5) 0.1390(4) 0.064(3) Uani 1.00 d . . . N(1**) N 1.2248(6) 1.2021(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . C(13**) C 1.3763(8) 1.2062(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14**) C 1.4154(8) 1.2078(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17**) C 1.4288(7) 1.0377(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18**) C 1.3791(7) 1.0359(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . C(9**) C 0.8112(9) 0.4529(5) 0.2682(4) 0.057(3) Uani 1.00 d . . . C(12**) C 0.8952(8) 0.4464(5) 0.1681(4) 0.067(4) Uani 1.00 d . . . C(8**) C 0.8856(7) 0.4243(4) 0.2361(4) 0.050(3) Uani 1.00 d . . . C(7**) C 0.9496(8) 0.3725(5) 0.2716(4) 0.057(3) Uani 1.00 d . . . C(6**) C 1.0283(8) 0.3563(5) 0.2496(4) 0.058(3) Uani 1.00 d . . . C(5**) C 1.0964(8) 0.3039(5) 0.2819(4) 0.053(3) Uani 1.00 d . . . C(1**) C 1.1681(8) 0.2813(5) 0.2445(4) 0.058(3) Uani 1.00 d . . . C(4**) C 1.0912(9) 0.2753(6) 0.3483(4) 0.070(4) Uani 1.00 d . . . C(2**) C 1.2292(8) 0.2296(5) 0.2721(4) 0.057(3) Uani 1.00 d . . . C(3**) C 1.1554(7) 0.2262(6) 0.3739(4) 0.061(3) Uani 1.00 d . . . N(1**) N 1.2248(6) 0.2021(3) 0.3360(3) 0.045(2) Uani 1.00 d . . . Rh(1**) Rh 1.31700(5) 0.11725(3) 0.37208(3) 0.0435(2) Uani 1.00 d . . . N(2'*) N 1.2379(6) 0.0258(3) 0.3283(3) 0.046(2) Uani 1.00 d . . . C(13**) C 1.3763(8) 0.2062(5) 0.4376(5) 0.064(4) Uani 1.00 d . . . C(14**) C 1.4154(8) 0.2078(5) 0.3756(6) 0.066(3) Uani 1.00 d . . . C(17**) C 1.4288(7) 0.0377(5) 0.3807(5) 0.059(3) Uani 1.00 d . . . C(18**) C 1.3791(7) 0.0359(5) 0.4399(5) 0.057(3) Uani 1.00 d . . . C(10'*) C 1.2474(7) 0.0029(5) 0.2649(4) 0.051(3) Uani 1.00 d . . . C(11'*) C 1.1683(8) -0.0021(5) 0.3610(4) 0.064(3) Uani 1.00 d . . . C(9'*) C 1.1888(9) -0.0471(5) 0.2318(4) 0.057(3) Uani 1.00 d . . . C(12'*) C 1.1048(8) -0.0536(5) 0.3319(4) 0.067(4) Uani 1.00 d . . . C(8'*) C 1.1144(7) -0.0757(4) 0.2639(4) 0.050(3) Uani 1.00 d . . . C(7'*) C 1.0504(8) -0.1275(5) 0.2284(4) 0.057(3) Uani 1.00 d . . . C(6'*) C 0.9717(8) -0.1437(5) 0.2504(4) 0.058(3) Uani 1.00 d . . . C(5'*) C 0.9036(8) -0.1961(5) 0.2181(4) 0.053(3) Uani 1.00 d . . . C(1'*) C 0.8319(8) -0.2187(5) 0.2555(4) 0.058(3) Uani 1.00 d . . . C(4'*) C 0.9088(9) -0.2247(6) 0.1517(4) 0.070(4) Uani 1.00 d . . . C(2'*) C 0.7708(8) -0.2704(5) 0.2279(4) 0.057(3) Uani 1.00 d . . . C(3'*) C 0.8446(7) -0.2738(6) 0.1261(4) 0.061(3) Uani 1.00 d . . . N(1'*) N 0.7752(6) -0.2979(3) 0.1640(3) 0.045(2) Uani 1.00 d . . . Rh(1'*) Rh 0.68300(5) -0.38275(3) 0.12792(3) 0.0435(2) Uani 1.00 d . . . N(2**) N 0.7621(6) -0.4742(3) 0.1717(3) 0.046(2) Uani 1.00 d . . . C(13'*) C 0.6237(8) -0.2938(5) 0.0624(5) 0.064(4) Uani 1.00 d . . . C(14'*) C 0.5846(8) -0.2922(5) 0.1244(6) 0.066(3) Uani 1.00 d . . . C(17'*) C 0.5712(7) -0.4623(5) 0.1193(5) 0.059(3) Uani 1.00 d . . . C(18'*) C 0.6209(7) -0.4641(5) 0.0601(5) 0.057(3) Uani 1.00 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0380(4) 0.0405(3) 0.0521(4) -0.0007(3) 0.0086(4) -0.0022(3) N(1) 0.043(6) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) N(2) 0.050(7) 0.040(3) 0.049(4) 0.013(3) 0.005(4) -0.002(3) C(1) 0.061(9) 0.066(5) 0.046(5) 0.009(5) 0.010(5) -0.006(4) C(2) 0.039(8) 0.065(5) 0.067(6) 0.007(5) 0.003(5) 0.000(4) C(3) 0.044(7) 0.093(6) 0.047(5) 0.026(5) -0.006(5) -0.014(5) C(4) 0.06(1) 0.088(6) 0.058(6) 0.019(6) -0.015(5) -0.013(5) C(5) 0.056(8) 0.055(5) 0.049(5) -0.005(4) 0.023(5) -0.005(4) C(6) 0.062(8) 0.058(5) 0.054(5) 0.006(5) 0.009(5) -0.012(4) C(7) 0.063(8) 0.059(5) 0.051(5) 0.013(5) -0.004(5) -0.016(4) C(8) 0.052(8) 0.046(4) 0.054(5) 0.008(4) 0.006(5) 0.005(4) C(9) 0.064(8) 0.060(5) 0.046(5) -0.001(5) 0.005(5) -0.004(4) C(10) 0.032(7) 0.070(5) 0.052(6) 0.009(5) -0.003(4) 0.002(4) C(11) 0.08(1) 0.077(6) 0.037(5) 0.022(5) -0.006(5) -0.009(4) C(12) 0.064(10) 0.089(6) 0.047(5) 0.042(6) -0.011(5) -0.023(4) C(13) 0.054(9) 0.060(5) 0.077(7) 0.000(5) 0.028(6) 0.018(5) C(14) 0.056(9) 0.051(5) 0.091(7) -0.018(4) 0.025(7) -0.006(5) C(17) 0.038(7) 0.052(4) 0.086(7) 0.017(4) 0.004(5) 0.007(5) C(18) 0.044(8) 0.051(5) 0.075(7) 0.010(4) 0.001(5) -0.011(4) N(2*) 0.050(7) 0.040(3) 0.049(4) -0.013(3) 0.005(4) 0.002(3) Rh(1*) 0.0380(4) 0.0405(3) 0.0521(4) 0.0007(3) 0.0086(4) 0.0022(3) C(10*) 0.032(7) 0.070(5) 0.052(6) -0.009(5) -0.003(4) -0.002(4) C(11*) 0.08(1) 0.077(6) 0.037(5) -0.022(5) -0.006(5) 0.009(4) N(1*) 0.043(6) 0.044(3) 0.047(4) 0.001(3) 0.004(4) 0.012(3) C(13*) 0.054(9) 0.060(5) 0.077(7) 0.000(5) 0.028(6) -0.018(5) C(14*) 0.056(9) 0.051(5) 0.091(7) 0.018(4) 0.025(7) 0.006(5) C(17*) 0.038(7) 0.052(4) 0.086(7) -0.017(4) 0.004(5) -0.007(5) C(18*) 0.044(8) 0.051(5) 0.075(7) -0.010(4) 0.001(5) 0.011(4) C(9*) 0.064(8) 0.060(5) 0.046(5) 0.001(5) 0.005(5) 0.004(4) C(12*) 0.064(10) 0.089(6) 0.047(5) -0.042(6) -0.011(5) 0.023(4) C(2*) 0.039(8) 0.065(5) 0.067(6) -0.007(5) 0.003(5) 0.000(4) C(3*) 0.044(7) 0.093(6) 0.047(5) -0.026(5) -0.006(5) 0.014(5) C(8*) 0.052(8) 0.046(4) 0.054(5) -0.008(4) 0.006(5) -0.005(4) C(1*) 0.061(9) 0.066(5) 0.046(5) -0.009(5) 0.010(5) 0.006(4) C(4*) 0.06(1) 0.088(6) 0.058(6) -0.019(6) -0.015(5) 0.013(5) C(7*) 0.063(8) 0.059(5) 0.051(5) -0.013(5) -0.004(5) 0.016(4) C(5*) 0.056(8) 0.055(5) 0.049(5) 0.005(4) 0.023(5) 0.005(4) C(6*) 0.062(8) 0.058(5) 0.054(5) -0.006(5) 0.009(5) 0.012(4) C(6*) 0.062(8) 0.058(5) 0.054(5) -0.006(5) 0.009(5) 0.012(4) C(5*) 0.056(8) 0.055(5) 0.049(5) 0.005(4) 0.023(5) 0.005(4) C(7*) 0.063(8) 0.059(5) 0.051(5) -0.013(5) -0.004(5) 0.016(4) C(1*) 0.061(9) 0.066(5) 0.046(5) -0.009(5) 0.010(5) 0.006(4) C(4*) 0.06(1) 0.088(6) 0.058(6) -0.019(6) -0.015(5) 0.013(5) C(8*) 0.052(8) 0.046(4) 0.054(5) -0.008(4) 0.006(5) -0.005(4) C(2*) 0.039(8) 0.065(5) 0.067(6) -0.007(5) 0.003(5) 0.000(4) C(3*) 0.044(7) 0.093(6) 0.047(5) -0.026(5) -0.006(5) 0.014(5) C(9*) 0.064(8) 0.060(5) 0.046(5) 0.001(5) 0.005(5) 0.004(4) C(12*) 0.064(10) 0.089(6) 0.047(5) -0.042(6) -0.011(5) 0.023(4) N(1*) 0.043(6) 0.044(3) 0.047(4) 0.001(3) 0.004(4) 0.012(3) C(10*) 0.032(7) 0.070(5) 0.052(6) -0.009(5) -0.003(4) -0.002(4) C(11*) 0.08(1) 0.077(6) 0.037(5) -0.022(5) -0.006(5) 0.009(4) Rh(1*) 0.0380(4) 0.0405(3) 0.0521(4) 0.0007(3) 0.0086(4) 0.0022(3) N(2*) 0.050(7) 0.040(3) 0.049(4) -0.013(3) 0.005(4) 0.002(3) N(2') 0.050(7) 0.040(3) 0.049(4) 0.013(3) 0.005(4) -0.002(3) C(13*) 0.054(9) 0.060(5) 0.077(7) 0.000(5) 0.028(6) -0.018(5) C(14*) 0.056(9) 0.051(5) 0.091(7) 0.018(4) 0.025(7) 0.006(5) C(17*) 0.038(7) 0.052(4) 0.086(7) -0.017(4) 0.004(5) -0.007(5) C(18*) 0.044(8) 0.051(5) 0.075(7) -0.010(4) 0.001(5) 0.011(4) Rh(1') 0.0380(4) 0.0405(3) 0.0521(4) -0.0007(3) 0.0086(4) -0.0022(3) N(1') 0.043(6) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) C(13') 0.054(9) 0.060(5) 0.077(7) 0.000(5) 0.028(6) 0.018(5) C(14') 0.056(9) 0.051(5) 0.091(7) -0.018(4) 0.025(7) -0.006(5) C(17') 0.038(7) 0.052(4) 0.086(7) 0.017(4) 0.004(5) 0.007(5) C(18') 0.044(8) 0.051(5) 0.075(7) 0.010(4) 0.001(5) -0.011(4) Rh(1*) 0.0429(4) 0.0441(3) 0.0468(4) -0.0006(3) 0.0036(4) -0.0121(3) N(1*) 0.043(6) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) N(2*) 0.043(7) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) C(1*) 0.043(9) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(2*) 0.043(8) 0.044(5) 0.047(6) -0.001(5) 0.004(5) -0.012(4) C(3*) 0.043(7) 0.044(6) 0.047(5) -0.001(5) 0.004(5) -0.012(5) C(4*) 0.04(1) 0.044(6) 0.047(6) -0.001(6) 0.004(5) -0.012(5) C(5*) 0.043(8) 0.044(5) 0.047(5) -0.001(4) 0.004(5) -0.012(4) C(6*) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(7*) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(8*) 0.043(8) 0.044(4) 0.047(5) -0.001(4) 0.004(5) -0.012(4) C(9*) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(10*) 0.043(7) 0.044(5) 0.047(6) -0.001(5) 0.004(4) -0.012(4) C(11*) 0.04(1) 0.044(6) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(12*) 0.043(10) 0.044(6) 0.047(5) -0.001(6) 0.004(5) -0.012(4) C(13*) 0.043(9) 0.044(5) 0.047(7) -0.001(5) 0.004(6) -0.012(5) C(14*) 0.043(9) 0.044(5) 0.047(7) -0.001(4) 0.004(7) -0.012(5) C(17*) 0.043(7) 0.044(4) 0.047(7) -0.001(4) 0.004(5) -0.012(5) C(18*) 0.043(8) 0.044(5) 0.047(7) -0.001(4) 0.004(5) -0.012(4) N(2**) 0.043(7) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) Rh(1**) 0.0429(4) 0.0441(3) 0.0468(4) -0.0006(3) 0.0036(4) -0.0121(3) C(10**) 0.043(7) 0.044(5) 0.047(6) -0.001(5) 0.004(4) -0.012(4) C(11**) 0.04(1) 0.044(6) 0.047(5) -0.001(5) 0.004(5) -0.012(4) N(1**) 0.043(6) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) C(13**) 0.043(9) 0.044(5) 0.047(7) -0.001(5) 0.004(6) -0.012(5) C(14**) 0.043(9) 0.044(5) 0.047(7) -0.001(4) 0.004(7) -0.012(5) C(17**) 0.043(7) 0.044(4) 0.047(7) -0.001(4) 0.004(5) -0.012(5) C(18**) 0.043(8) 0.044(5) 0.047(7) -0.001(4) 0.004(5) -0.012(4) C(9**) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(12**) 0.043(10) 0.044(6) 0.047(5) -0.001(6) 0.004(5) -0.012(4) C(2**) 0.043(8) 0.044(5) 0.047(6) -0.001(5) 0.004(5) -0.012(4) C(3**) 0.043(7) 0.044(6) 0.047(5) -0.001(5) 0.004(5) -0.012(5) C(8**) 0.043(8) 0.044(4) 0.047(5) -0.001(4) 0.004(5) -0.012(4) C(1**) 0.043(9) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(4**) 0.04(1) 0.044(6) 0.047(6) -0.001(6) 0.004(5) -0.012(5) C(7**) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(5**) 0.043(8) 0.044(5) 0.047(5) -0.001(4) 0.004(5) -0.012(4) C(6**) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(6**) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(5**) 0.043(8) 0.044(5) 0.047(5) -0.001(4) 0.004(5) -0.012(4) C(7**) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(1**) 0.043(9) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(4**) 0.04(1) 0.044(6) 0.047(6) -0.001(6) 0.004(5) -0.012(5) C(8**) 0.043(8) 0.044(4) 0.047(5) -0.001(4) 0.004(5) -0.012(4) C(2**) 0.043(8) 0.044(5) 0.047(6) -0.001(5) 0.004(5) -0.012(4) C(3**) 0.043(7) 0.044(6) 0.047(5) -0.001(5) 0.004(5) -0.012(5) C(9**) 0.043(8) 0.044(5) 0.047(5) -0.001(5) 0.004(5) -0.012(4) C(12**) 0.043(10) 0.044(6) 0.047(5) -0.001(6) 0.004(5) -0.012(4) N(1**) 0.043(6) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) C(10**) 0.043(7) 0.044(5) 0.047(6) -0.001(5) 0.004(4) -0.012(4) C(11**) 0.04(1) 0.044(6) 0.047(5) -0.001(5) 0.004(5) -0.012(4) Rh(1**) 0.0429(4) 0.0441(3) 0.0468(4) -0.0006(3) 0.0036(4) -0.0121(3) N(2**) 0.043(7) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) N(2'*) 0.043(7) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) C(13**) 0.043(9) 0.044(5) 0.047(7) -0.001(5) 0.004(6) -0.012(5) C(14**) 0.043(9) 0.044(5) 0.047(7) -0.001(4) 0.004(7) -0.012(5) C(17**) 0.043(7) 0.044(4) 0.047(7) -0.001(4) 0.004(5) -0.012(5) C(18**) 0.043(8) 0.044(5) 0.047(7) -0.001(4) 0.004(5) -0.012(4) Rh(1'*) 0.0429(4) 0.0441(3) 0.0468(4) -0.0006(3) 0.0036(4) -0.0121(3) N(1'*) 0.043(6) 0.044(3) 0.047(4) -0.001(3) 0.004(4) -0.012(3) C(13'*) 0.043(9) 0.044(5) 0.047(7) -0.001(5) 0.004(6) -0.012(5) C(14'*) 0.043(9) 0.044(5) 0.047(7) -0.001(4) 0.004(7) -0.012(5) C(17'*) 0.043(7) 0.044(4) 0.047(7) -0.001(4) 0.004(5) -0.012(5) C(18'*) 0.043(8) 0.044(5) 0.047(7) -0.001(4) 0.004(5) -0.012(4) Rh(1*) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) N(1*) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) N(2*) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(1*) 0.043(9) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(2*) 0.043(8) 0.044(5) 0.047(6) 0.001(5) -0.004(5) -0.012(4) C(3*) 0.043(7) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(5) C(4*) 0.04(1) 0.044(6) 0.047(6) 0.001(6) -0.004(5) -0.012(5) C(5*) 0.043(8) 0.044(5) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(6*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(7*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(8*) 0.043(8) 0.044(4) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(9*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(10*) 0.043(7) 0.044(5) 0.047(6) 0.001(5) -0.004(4) -0.012(4) C(11*) 0.04(1) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(12*) 0.043(10) 0.044(6) 0.047(5) 0.001(6) -0.004(5) -0.012(4) C(13*) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14*) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17*) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18*) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) N(2**) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) Rh(1**) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) C(10**) 0.043(7) 0.044(5) 0.047(6) 0.001(5) -0.004(4) -0.012(4) C(11**) 0.04(1) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(4) N(1**) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(13**) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14**) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17**) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18**) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) C(9**) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(12**) 0.043(10) 0.044(6) 0.047(5) 0.001(6) -0.004(5) -0.012(4) C(8**) 0.043(8) 0.044(4) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(7**) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(6**) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(5**) 0.043(8) 0.044(5) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(1**) 0.043(9) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(4**) 0.04(1) 0.044(6) 0.047(6) 0.001(6) -0.004(5) -0.012(5) C(2**) 0.043(8) 0.044(5) 0.047(6) 0.001(5) -0.004(5) -0.012(4) C(3**) 0.043(7) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(5) N(1**) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) Rh(1**) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) N(2'*) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(13**) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14**) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17**) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18**) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) C(10'*) 0.043(7) 0.044(5) 0.047(6) 0.001(5) -0.004(4) -0.012(4) C(11'*) 0.04(1) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(9'*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(12'*) 0.043(10) 0.044(6) 0.047(5) 0.001(6) -0.004(5) -0.012(4) C(8'*) 0.043(8) 0.044(4) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(7'*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(6'*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(5'*) 0.043(8) 0.044(5) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(1'*) 0.043(9) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(4'*) 0.04(1) 0.044(6) 0.047(6) 0.001(6) -0.004(5) -0.012(5) C(2'*) 0.043(8) 0.044(5) 0.047(6) 0.001(5) -0.004(5) -0.012(4) C(3'*) 0.043(7) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(5) N(1'*) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) Rh(1'*) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) N(2**) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(13'*) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14'*) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17'*) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18'*) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) Rh(1*) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) N(1*) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) N(2*) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(1*) 0.043(9) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(2*) 0.043(8) 0.044(5) 0.047(6) 0.001(5) -0.004(5) -0.012(4) C(3*) 0.043(7) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(5) C(4*) 0.04(1) 0.044(6) 0.047(6) 0.001(6) -0.004(5) -0.012(5) C(5*) 0.043(8) 0.044(5) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(6*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(7*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(8*) 0.043(8) 0.044(4) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(9*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(10*) 0.043(7) 0.044(5) 0.047(6) 0.001(5) -0.004(4) -0.012(4) C(11*) 0.04(1) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(12*) 0.043(10) 0.044(6) 0.047(5) 0.001(6) -0.004(5) -0.012(4) C(13*) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14*) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17*) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18*) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) N(2**) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) Rh(1**) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) C(10**) 0.043(7) 0.044(5) 0.047(6) 0.001(5) -0.004(4) -0.012(4) C(11**) 0.04(1) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(4) N(1**) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(13**) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14**) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17**) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18**) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) C(9**) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(12**) 0.043(10) 0.044(6) 0.047(5) 0.001(6) -0.004(5) -0.012(4) C(8**) 0.043(8) 0.044(4) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(7**) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(6**) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(5**) 0.043(8) 0.044(5) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(1**) 0.043(9) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(4**) 0.04(1) 0.044(6) 0.047(6) 0.001(6) -0.004(5) -0.012(5) C(2**) 0.043(8) 0.044(5) 0.047(6) 0.001(5) -0.004(5) -0.012(4) C(3**) 0.043(7) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(5) N(1**) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) Rh(1**) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) N(2'*) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(13**) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14**) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17**) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18**) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) C(10'*) 0.043(7) 0.044(5) 0.047(6) 0.001(5) -0.004(4) -0.012(4) C(11'*) 0.04(1) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(9'*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(12'*) 0.043(10) 0.044(6) 0.047(5) 0.001(6) -0.004(5) -0.012(4) C(8'*) 0.043(8) 0.044(4) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(7'*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(6'*) 0.043(8) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(5'*) 0.043(8) 0.044(5) 0.047(5) 0.001(4) -0.004(5) -0.012(4) C(1'*) 0.043(9) 0.044(5) 0.047(5) 0.001(5) -0.004(5) -0.012(4) C(4'*) 0.04(1) 0.044(6) 0.047(6) 0.001(6) -0.004(5) -0.012(5) C(2'*) 0.043(8) 0.044(5) 0.047(6) 0.001(5) -0.004(5) -0.012(4) C(3'*) 0.043(7) 0.044(6) 0.047(5) 0.001(5) -0.004(5) -0.012(5) N(1'*) 0.043(6) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) Rh(1'*) 0.0429(4) 0.0441(3) 0.0468(4) 0.0006(3) -0.0036(4) -0.0121(3) N(2**) 0.043(7) 0.044(3) 0.047(4) 0.001(3) -0.004(4) -0.012(3) C(13'*) 0.043(9) 0.044(5) 0.047(7) 0.001(5) -0.004(6) -0.012(5) C(14'*) 0.043(9) 0.044(5) 0.047(7) 0.001(4) -0.004(7) -0.012(5) C(17'*) 0.043(7) 0.044(4) 0.047(7) 0.001(4) -0.004(5) -0.012(5) C(18'*) 0.043(8) 0.044(5) 0.047(7) 0.001(4) -0.004(5) -0.012(4) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) N(1) 2.101(7) . . yes Rh(1) N(2) 2.108(6) . 3_645 yes Rh(1) C(13) 2.149(8) . . yes Rh(1) C(14) 2.111(9) . . yes Rh(1) C(17) 2.148(9) . . yes Rh(1) C(18) 2.112(8) . . yes F(1) B(1) 1.26(1) . . yes F(2) B(1) 1.18(1) . . yes F(3) B(1) 1.34(1) . . yes F(4) B(1) 1.36(2) . . yes O(1) C(22) 1.22(2) . . yes N(1) C(2) 1.339(10) . . yes N(1) C(3) 1.35(1) . . yes N(2) C(10) 1.313(10) . . yes N(2) C(11) 1.32(1) . . yes C(1) C(2) 1.37(1) . . yes C(1) C(5) 1.37(1) . . yes C(3) C(4) 1.36(1) . . yes C(4) C(5) 1.39(1) . . yes C(5) C(6) 1.49(1) . . yes C(6) C(7) 1.30(1) . . yes C(7) C(8) 1.47(1) . . yes C(8) C(9) 1.38(1) . . yes C(8) C(12) 1.40(1) . . yes C(9) C(10) 1.38(1) . . yes C(11) C(12) 1.41(1) . . yes C(13) C(14) 1.36(1) . . yes C(13) C(20) 1.47(1) . . yes C(14) C(15) 1.53(2) . . yes C(15) C(16) 1.45(2) . . yes C(16) C(17) 1.53(1) . . yes C(17) C(18) 1.39(1) . . yes C(18) C(19) 1.51(1) . . yes C(19) C(20) 1.49(1) . . yes C(21) C(22) 1.45(3) . . yes C(22) C(23) 1.48(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Rh(1) N(2) 87.6(3) . 1_555 3_645 yes N(1) Rh(1) C(13) 91.6(3) . 1_555 1_555 yes N(1) Rh(1) C(14) 90.6(3) . 1_555 1_555 yes N(1) Rh(1) C(17) 163.2(3) . 1_555 1_555 yes N(1) Rh(1) C(18) 158.8(3) . 1_555 1_555 yes N(2) Rh(1) C(13) 165.9(4) . 3_645 1_555 yes N(2) Rh(1) C(14) 156.9(4) . 3_645 1_555 yes N(2) Rh(1) C(17) 92.6(3) . 3_645 1_555 yes N(2) Rh(1) C(18) 93.4(3) . 3_645 1_555 yes C(13) Rh(1) C(14) 37.2(4) . 1_555 1_555 yes C(13) Rh(1) C(17) 92.2(4) . 1_555 1_555 yes C(13) Rh(1) C(18) 82.3(3) . 1_555 1_555 yes C(14) Rh(1) C(17) 82.6(4) . 1_555 1_555 yes C(14) Rh(1) C(18) 96.5(4) . 1_555 1_555 yes C(17) Rh(1) C(18) 38.0(3) . 1_555 1_555 yes Rh(1) N(1) C(2) 120.6(6) . 1_555 1_555 yes Rh(1) N(1) C(3) 121.8(5) . 1_555 1_555 yes C(2) N(1) C(3) 117.4(8) . 1_555 1_555 yes Rh(1) N(2) C(10) 122.1(6) . 3_655 1_555 yes Rh(1) N(2) C(11) 120.3(5) . 3_655 1_555 yes C(10) N(2) C(11) 116.9(7) . 1_555 1_555 yes C(2) C(1) C(5) 119.5(8) . 1_555 1_555 yes N(1) C(2) C(1) 123.3(9) . 1_555 1_555 yes N(1) C(3) C(4) 121.7(8) . 1_555 1_555 yes C(3) C(4) C(5) 120.6(10) . 1_555 1_555 yes C(1) C(5) C(4) 117.4(8) . 1_555 1_555 yes C(1) C(5) C(6) 118.7(8) . 1_555 1_555 yes C(4) C(5) C(6) 123.9(10) . 1_555 1_555 yes C(5) C(6) C(7) 127.9(9) . 1_555 1_555 yes C(6) C(7) C(8) 124.5(8) . 1_555 1_555 yes C(7) C(8) C(9) 121.4(8) . 1_555 1_555 yes C(7) C(8) C(12) 122.7(9) . 1_555 1_555 yes C(9) C(8) C(12) 115.9(8) . 1_555 1_555 yes C(8) C(9) C(10) 121.0(8) . 1_555 1_555 yes N(2) C(10) C(9) 123.6(8) . 1_555 1_555 yes N(2) C(11) C(12) 124.0(7) . 1_555 1_555 yes C(8) C(12) C(11) 118.6(9) . 1_555 1_555 yes Rh(1) C(13) C(14) 69.9(5) . 1_555 1_555 yes Rh(1) C(13) C(20) 111.5(6) . 1_555 1_555 yes C(14) C(13) C(20) 126(1) . 1_555 1_555 yes Rh(1) C(14) C(13) 73.0(6) . 1_555 1_555 yes Rh(1) C(14) C(15) 110.0(6) . 1_555 1_555 yes C(13) C(14) C(15) 128.1(10) . 1_555 1_555 yes C(14) C(15) C(16) 114.0(10) . 1_555 1_555 yes C(15) C(16) C(17) 116(1) . 1_555 1_555 yes Rh(1) C(17) C(16) 109.7(6) . 1_555 1_555 yes Rh(1) C(17) C(18) 69.6(6) . 1_555 1_555 yes C(16) C(17) C(18) 124.8(9) . 1_555 1_555 yes Rh(1) C(18) C(17) 72.4(5) . 1_555 1_555 yes Rh(1) C(18) C(19) 110.8(5) . 1_555 1_555 yes C(17) C(18) C(19) 123(1) . 1_555 1_555 yes C(18) C(19) C(20) 115.5(8) . 1_555 1_555 yes C(13) C(20) C(19) 116.5(8) . 1_555 1_555 yes O(1) C(22) C(21) 122(1) . 1_555 1_555 yes O(1) C(22) C(23) 117(2) . 1_555 1_555 yes C(21) C(22) C(23) 119(1) . 1_555 1_555 yes F(1) B(1) F(2) 116(1) . 1_555 1_555 yes F(1) B(1) F(3) 112(1) . 1_555 1_555 yes F(1) B(1) F(4) 95(1) . 1_555 1_555 yes F(2) B(1) F(3) 115(1) . 1_555 1_555 yes F(2) B(1) F(4) 104(1) . 1_555 1_555 yes F(3) B(1) F(4) 110(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Rh(1) F(3) 3.509(7) . 8_555 ? F(1) C(9) 3.27(1) . 7_555 ? F(1) C(1) 3.39(1) . 2_456 ? F(1) C(21) 3.52(2) . 4_655 ? F(1) C(22) 3.53(2) . 4_655 ? F(1) C(6) 3.54(2) . 2_456 ? F(1) C(10) 3.58(1) . 7_555 ? F(2) C(21) 3.42(2) . 7_455 ? F(3) C(11) 3.156(9) . 6_545 ? F(3) C(3) 3.44(1) . 8_455 ? F(3) C(18) 3.59(1) . 8_455 ? F(4) C(23) 3.32(2) . 8_355 ? F(4) C(12) 3.49(2) . 2_456 ? F(4) C(6) 3.53(1) . 2_456 ? F(4) C(15) 3.53(2) . 7_455 ? F(4) C(14) 3.53(1) . 7_455 ? O(1) C(2) 3.39(2) . 8_555 ? N(2) C(18) 3.07(1) . 3_655 ? N(2) C(17) 3.08(1) . 3_655 ? N(2) C(2) 3.54(1) . 3_655 ? C(1) C(9) 3.57(1) . 8_555 ? #------------------------------------------------------------------------------ #===END