# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yasushi Mizobe' _publ_contact_author_email YMIZOBE@IIS.U-TOKYO.AC.JP _publ_section_title ; Heterolytic H2 Activation by Rhodium Thiolato Complexes Bearing Hydrotris(pyrazolyl)borato Ligand and its Application to Catalytic Hydrogenation under Mild Conditions ; loop_ _publ_author_name 'Yasushi Mizobe' 'Yoshihiro Hojo' 'Yoshiyuki Misumi' 'Hidetake Seino' # Attachment 'CIF-TpsRh1.txt' #TrackingRef 'CIF-TpsRh1.txt' data___[TpMe2Rh(S2C6H4)(MeCN)]_2THF _database_code_depnum_ccdc_archive 'CCDC 753657' #TrackingRef 'CIF-TpsRh1.txt' _audit_creation_date 2009-08-09 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C31 H45 B N7 O2 Rh S2 ' _chemical_formula_moiety 'C31 H45 B N7 O2 Rh S2 ' _chemical_formula_weight 725.58 _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 10.1804(15) _cell_length_b 22.607(4) _cell_length_c 14.737(2) _cell_angle_alpha 90.0000 _cell_angle_beta 91.2870(7) _cell_angle_gamma 90.0000 _cell_volume 3390.8(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9749 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512.00 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.936 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_ambient_temperature 113.1 _diffrn_reflns_number 35590 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.88 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #============================================================================== # 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 8065 _reflns_number_gt 6356 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1228 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 8065 _refine_ls_number_parameters 528 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.5000\s(Fo^2^) + 0.1000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0027 _refine_diff_density_max 1.82 _refine_diff_density_min -1.45 _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) ; B B 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; 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) ; #============================================================================== # 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 Rh(1) Rh 0.56156(2) 0.191660(10) 0.45276(2) 0.02029(6) Uani 1.00 1 d . . . S(1) S 0.34477(8) 0.19886(4) 0.49648(6) 0.0275(2) Uani 1.00 1 d . . . S(2) S 0.53651(8) 0.28239(4) 0.38154(5) 0.02673(19) Uani 1.00 1 d . . . O(1) O 0.8364(3) 0.05032(18) 0.9840(2) 0.0799(13) Uani 1.00 1 d . . . O(2) O 0.9349(7) 0.1729(4) 0.7308(5) 0.077(2) Uani 0.50 1 d P . . O(3) O 0.9859(7) 0.2000(2) 0.6821(5) 0.057(2) Uani 0.50 1 d P . . N(1) N 0.8018(2) 0.13013(12) 0.38433(17) 0.0242(6) Uani 1.00 1 d . . . N(2) N 0.7621(2) 0.18479(11) 0.41556(17) 0.0212(6) Uani 1.00 1 d . . . N(3) N 0.6508(2) 0.06638(11) 0.47447(17) 0.0236(6) Uani 1.00 1 d . . . N(4) N 0.5885(2) 0.11045(11) 0.52085(17) 0.0240(6) Uani 1.00 1 d . . . N(5) N 0.5867(2) 0.09823(11) 0.31585(16) 0.0230(6) Uani 1.00 1 d . . . N(6) N 0.5094(2) 0.14600(12) 0.33671(17) 0.0233(6) Uani 1.00 1 d . . . N(7) N 0.6212(2) 0.23542(12) 0.56401(17) 0.0248(6) Uani 1.00 1 d . . . C(1) C 0.8676(3) 0.21988(15) 0.4166(2) 0.0285(8) Uani 1.00 1 d . . . C(2) C 0.9749(3) 0.18859(16) 0.3854(2) 0.0323(9) Uani 1.00 1 d . . . C(3) C 0.9315(3) 0.13234(16) 0.3654(2) 0.0297(8) Uani 1.00 1 d . . . C(4) C 0.8648(3) 0.28303(17) 0.4482(3) 0.0391(10) Uani 1.00 1 d . . . C(5) C 1.0041(4) 0.0812(2) 0.3270(3) 0.0433(11) Uani 1.00 1 d . . . C(6) C 0.5659(3) 0.08993(15) 0.6041(2) 0.0276(8) Uani 1.00 1 d . . . C(7) C 0.6126(3) 0.03211(15) 0.6115(2) 0.0280(8) Uani 1.00 1 d . . . C(8) C 0.6665(3) 0.01819(14) 0.5292(2) 0.0261(7) Uani 1.00 1 d . . . C(9) C 0.5014(4) 0.12588(18) 0.6757(2) 0.0359(9) Uani 1.00 1 d . . . C(10) C 0.7302(4) -0.03698(16) 0.4988(2) 0.0346(9) Uani 1.00 1 d . . . C(11) C 0.4237(2) 0.15371(15) 0.2664(2) 0.0258(7) Uani 1.00 1 d . . . C(12) C 0.4479(3) 0.11062(16) 0.2010(2) 0.0314(8) Uani 1.00 1 d . . . C(13) C 0.5509(3) 0.07686(15) 0.2332(2) 0.0279(7) Uani 1.00 1 d . . . C(14) C 0.3213(3) 0.2011(2) 0.2597(2) 0.0344(10) Uani 1.00 1 d . . . C(15) C 0.6191(4) 0.02612(19) 0.1890(2) 0.0399(11) Uani 1.00 1 d . . . C(16) C 0.3116(3) 0.27496(15) 0.4822(2) 0.0261(7) Uani 1.00 1 d . . . C(17) C 0.3944(3) 0.31127(14) 0.4317(2) 0.0256(7) Uani 1.00 1 d . . . C(18) C 0.3632(3) 0.37118(16) 0.4214(2) 0.0314(8) Uani 1.00 1 d . . . C(19) C 0.2520(3) 0.39480(17) 0.4597(2) 0.0338(9) Uani 1.00 1 d . . . C(20) C 0.1701(3) 0.35884(17) 0.5095(2) 0.0341(9) Uani 1.00 1 d . . . C(21) C 0.1996(3) 0.29948(16) 0.5205(2) 0.0305(8) Uani 1.00 1 d . . . C(22) C 0.6675(3) 0.26035(14) 0.6223(2) 0.0260(7) Uani 1.00 1 d . . . C(23) C 0.7340(4) 0.2918(2) 0.6970(2) 0.0417(11) Uani 1.00 1 d . . . C(24) C 0.7037(5) 0.0618(2) 0.9550(3) 0.0733(18) Uani 1.00 1 d . . . C(25) C 0.7107(5) 0.0619(2) 0.8565(3) 0.0745(18) Uani 1.00 1 d . . . C(26) C 0.8156(5) 0.0210(2) 0.8346(4) 0.0795(19) Uani 1.00 1 d . . . C(27) C 0.9153(6) 0.0337(3) 0.9110(5) 0.117(3) Uani 1.00 1 d . . . C(28) C 0.9032(4) 0.1506(2) 0.6462(3) 0.0567(13) Uani 1.00 1 d . . . C(29) C 1.0022(5) 0.1052(2) 0.6241(4) 0.0717(16) Uani 1.00 1 d . . . C(30) C 1.1151(9) 0.1159(4) 0.6920(7) 0.045(2) Uiso 0.50 1 d P . . C(31) C 1.0771(11) 0.1719(5) 0.7422(8) 0.056(3) Uiso 0.50 1 d P . . C(32) C 1.0920(12) 0.1060(5) 0.7179(8) 0.067(3) Uiso 0.50 1 d P . . C(33) C 1.1073(10) 0.1758(5) 0.7189(7) 0.050(2) Uiso 0.50 1 d P . . B(1) B 0.7017(3) 0.07865(16) 0.3790(2) 0.0242(8) Uani 1.00 1 d . . . H(1) H 0.752(3) 0.0379(14) 0.351(2) 0.023(8) Uiso 1.00 1 c . . . H(2) H 1.056(3) 0.2025(15) 0.384(2) 0.026(9) Uiso 1.00 1 c . . . H(3) H 0.766(4) 0.303(2) 0.448(3) 0.066(14) Uiso 1.00 1 c . . . H(4) H 0.934(4) 0.3036(19) 0.413(3) 0.060(14) Uiso 1.00 1 c . . . H(5) H 0.912(5) 0.295(2) 0.526(4) 0.10(2) Uiso 1.00 1 c . . . H(6) H 0.976(4) 0.0658(19) 0.266(3) 0.052(12) Uiso 1.00 1 c . . . H(7) H 1.009(3) 0.0512(18) 0.365(2) 0.037(10) Uiso 1.00 1 c . . . H(8) H 1.105(4) 0.094(2) 0.314(2) 0.060(13) Uiso 1.00 1 c . . . H(9) H 0.610(3) 0.0070(17) 0.661(2) 0.033(9) Uiso 1.00 1 c . . . H(10) H 0.420(7) 0.159(3) 0.646(5) 0.14(2) Uiso 1.00 1 c . . . H(11) H 0.567(4) 0.1378(19) 0.709(2) 0.045(12) Uiso 1.00 1 c . . . H(12) H 0.447(4) 0.101(2) 0.717(3) 0.057(12) Uiso 1.00 1 c . . . H(13) H 0.686(3) -0.0557(16) 0.444(2) 0.033(9) Uiso 1.00 1 c . . . H(14) H 0.725(4) -0.065(2) 0.546(3) 0.059(13) Uiso 1.00 1 c . . . H(15) H 0.828(4) -0.0362(19) 0.495(2) 0.051(12) Uiso 1.00 1 c . . . H(16) H 0.408(3) 0.1045(17) 0.148(2) 0.037(10) Uiso 1.00 1 c . . . H(17) H 0.301(4) 0.2136(19) 0.316(3) 0.049(12) Uiso 1.00 1 c . . . H(18) H 0.238(4) 0.1841(18) 0.225(3) 0.054(12) Uiso 1.00 1 c . . . H(19) H 0.353(4) 0.222(2) 0.229(3) 0.053(14) Uiso 1.00 1 c . . . H(20) H 0.620(4) 0.001(2) 0.224(3) 0.058(14) Uiso 1.00 1 c . . . H(21) H 0.717(4) 0.040(2) 0.174(3) 0.061(13) Uiso 1.00 1 c . . . H(22) H 0.574(3) 0.0207(18) 0.128(3) 0.048(11) Uiso 1.00 1 c . . . H(23) H 0.421(3) 0.3934(17) 0.389(2) 0.034(10) Uiso 1.00 1 c . . . H(24) H 0.234(3) 0.4362(18) 0.453(2) 0.040(10) Uiso 1.00 1 c . . . H(25) H 0.090(4) 0.373(2) 0.536(3) 0.068(14) Uiso 1.00 1 c . . . H(26) H 0.141(3) 0.2747(18) 0.556(2) 0.040(10) Uiso 1.00 1 c . . . H(27) H 0.809(5) 0.272(2) 0.704(3) 0.083(17) Uiso 1.00 1 c . . . H(28) H 0.674(5) 0.290(2) 0.748(3) 0.070(15) Uiso 1.00 1 c . . . H(29) H 0.761(5) 0.332(2) 0.677(3) 0.080(17) Uiso 1.00 1 c . . . H(30) H 0.6466 0.0316 0.9754 0.088 Uiso 1.00 1 c R . . H(31) H 0.6746 0.0990 0.9767 0.088 Uiso 1.00 1 c R . . H(32) H 0.6301 0.0484 0.8302 0.090 Uiso 1.00 1 c R . . H(33) H 0.7289 0.1006 0.8351 0.090 Uiso 1.00 1 c R . . H(34) H 0.7882 -0.0191 0.8366 0.095 Uiso 1.00 1 c R . . H(35) H 0.8492 0.0295 0.7764 0.095 Uiso 1.00 1 c R . . H(36) H 0.9693 0.0660 0.8944 0.141 Uiso 1.00 1 c R . . H(37) H 0.9688 0.0002 0.9240 0.141 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 Rh(1) 0.02276(14) 0.02275(14) 0.01530(13) -0.00533(9) -0.00096(9) 0.00208(8) S(1) 0.0258(4) 0.0298(4) 0.0271(4) -0.0039(3) 0.0047(3) 0.0049(3) S(2) 0.0280(3) 0.0271(4) 0.0252(3) -0.0037(3) 0.0017(3) 0.0068(3) O(1) 0.073(2) 0.078(2) 0.087(2) -0.003(2) -0.034(2) 0.014(2) O(2) 0.065(4) 0.091(6) 0.073(5) 0.042(4) -0.028(4) -0.045(4) O(3) 0.063(4) 0.035(3) 0.075(5) 0.015(2) 0.010(3) -0.000(3) N(1) 0.0246(12) 0.0294(14) 0.0184(12) -0.0018(10) -0.0027(10) 0.0014(10) N(2) 0.0206(12) 0.0263(13) 0.0166(11) -0.0017(9) -0.0028(9) 0.0010(9) N(3) 0.0269(12) 0.0235(12) 0.0203(12) -0.0037(10) -0.0009(10) 0.0028(10) N(4) 0.0299(13) 0.0242(13) 0.0180(12) -0.0049(10) 0.0009(10) 0.0005(9) N(5) 0.0280(13) 0.0249(13) 0.0162(11) -0.0064(10) 0.0004(9) 0.0024(9) N(6) 0.0237(12) 0.0285(13) 0.0176(11) -0.0073(10) -0.0003(9) 0.0011(10) N(7) 0.0279(13) 0.0268(13) 0.0196(12) -0.0001(10) -0.0002(10) -0.0001(10) C(1) 0.0241(15) 0.0337(18) 0.0275(16) -0.0063(13) -0.0045(12) 0.0054(13) C(2) 0.0219(16) 0.042(2) 0.0332(18) -0.0099(14) 0.0006(13) 0.0037(14) C(3) 0.0269(16) 0.0373(18) 0.0250(16) -0.0001(13) 0.0006(12) 0.0040(13) C(4) 0.0318(19) 0.0324(19) 0.053(2) -0.0129(15) 0.0015(17) -0.0023(17) C(5) 0.036(2) 0.048(2) 0.046(2) 0.0038(18) 0.0059(18) -0.001(2) C(6) 0.0317(16) 0.0303(16) 0.0206(14) -0.0057(13) 0.0012(12) 0.0050(12) C(7) 0.0311(16) 0.0287(16) 0.0240(15) -0.0084(13) -0.0018(13) 0.0072(13) C(8) 0.0288(15) 0.0262(15) 0.0230(15) -0.0066(12) -0.0069(12) 0.0048(12) C(9) 0.049(2) 0.040(2) 0.0195(16) -0.0005(17) 0.0090(16) 0.0050(14) C(10) 0.043(2) 0.0269(17) 0.0337(19) 0.0006(15) -0.0082(16) 0.0025(14) C(11) 0.0232(14) 0.0330(17) 0.0210(14) -0.0092(12) -0.0024(11) 0.0037(12) C(12) 0.0369(18) 0.0382(19) 0.0187(15) -0.0097(15) -0.0069(13) 0.0005(13) C(13) 0.0360(16) 0.0292(16) 0.0184(14) -0.0115(13) 0.0013(12) -0.0006(12) C(14) 0.0282(18) 0.052(2) 0.0229(18) -0.0031(16) -0.0035(14) 0.0035(16) C(15) 0.061(2) 0.034(2) 0.0242(18) 0.0007(18) -0.0004(18) -0.0037(15) C(16) 0.0270(15) 0.0320(17) 0.0192(14) -0.0046(13) -0.0045(12) 0.0007(12) C(17) 0.0253(15) 0.0302(16) 0.0211(15) -0.0046(12) -0.0057(12) 0.0010(12) C(18) 0.0317(17) 0.0324(18) 0.0298(17) -0.0044(14) -0.0058(14) 0.0056(14) C(19) 0.0332(17) 0.0322(18) 0.0357(19) 0.0003(14) -0.0100(14) 0.0006(14) C(20) 0.0273(16) 0.041(2) 0.0341(18) 0.0023(15) -0.0051(14) -0.0029(15) C(21) 0.0255(16) 0.0403(19) 0.0255(16) -0.0028(13) -0.0026(13) -0.0002(14) C(22) 0.0257(15) 0.0272(16) 0.0250(15) 0.0069(12) -0.0001(12) -0.0015(12) C(23) 0.040(2) 0.052(2) 0.033(2) 0.0093(19) -0.0086(17) -0.0209(18) C(24) 0.075(3) 0.071(3) 0.074(3) 0.008(2) -0.012(2) 0.016(2) C(25) 0.086(3) 0.073(3) 0.065(3) -0.001(3) 0.018(2) -0.007(2) C(26) 0.070(3) 0.073(3) 0.095(4) -0.007(2) -0.011(3) -0.007(3) C(27) 0.071(4) 0.145(7) 0.135(6) -0.033(4) 0.025(4) -0.052(5) C(28) 0.051(2) 0.063(3) 0.056(2) 0.008(2) -0.013(2) -0.005(2) C(29) 0.066(3) 0.058(3) 0.090(3) 0.021(2) -0.031(2) -0.023(2) B(1) 0.0272(16) 0.0278(17) 0.0175(15) -0.0041(14) -0.0003(13) 0.0012(13) #============================================================================== _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 Rh(1) S(1) 2.3187(8) yes . . Rh(1) S(2) 2.3155(9) yes . . Rh(1) N(2) 2.132(2) yes . . Rh(1) N(4) 2.107(2) yes . . Rh(1) N(6) 2.057(2) yes . . Rh(1) N(7) 1.998(2) yes . . S(1) C(16) 1.765(3) yes . . S(2) C(17) 1.765(3) yes . . O(1) C(24) 1.431(6) yes . . O(1) C(27) 1.408(8) yes . . O(2) C(28) 1.377(9) yes . . O(2) C(31) 1.454(14) yes . . O(3) C(28) 1.489(8) yes . . O(3) C(33) 1.446(13) yes . . N(1) N(2) 1.382(3) yes . . N(1) C(3) 1.357(4) yes . . N(1) B(1) 1.548(4) yes . . N(2) C(1) 1.335(4) yes . . N(3) N(4) 1.371(3) yes . . N(3) C(8) 1.363(4) yes . . N(3) B(1) 1.536(4) yes . . N(4) C(6) 1.336(4) yes . . N(5) N(6) 1.375(3) yes . . N(5) C(13) 1.353(3) yes . . N(5) B(1) 1.543(4) yes . . N(6) C(11) 1.351(3) yes . . N(7) C(22) 1.122(4) yes . . C(1) C(2) 1.388(4) yes . . C(1) C(4) 1.502(5) yes . . C(2) C(3) 1.376(5) yes . . C(3) C(5) 1.490(5) yes . . C(6) C(7) 1.394(4) yes . . C(6) C(9) 1.496(5) yes . . C(7) C(8) 1.378(4) yes . . C(8) C(10) 1.480(4) yes . . C(11) C(12) 1.396(4) yes . . C(11) C(14) 1.496(5) yes . . C(12) C(13) 1.373(4) yes . . C(13) C(15) 1.497(5) yes . . C(16) C(17) 1.402(4) yes . . C(16) C(21) 1.398(4) yes . . C(17) C(18) 1.399(4) yes . . C(18) C(19) 1.383(5) yes . . C(19) C(20) 1.386(5) yes . . C(20) C(21) 1.384(5) yes . . C(22) C(23) 1.464(5) yes . . C(24) C(25) 1.456(7) yes . . C(25) C(26) 1.454(8) yes . . C(26) C(27) 1.526(9) yes . . C(28) C(29) 1.480(7) yes . . C(29) C(30) 1.526(11) yes . . C(29) C(32) 1.640(14) yes . . C(30) C(31) 1.521(15) yes . . C(30) C(33) 1.414(15) yes . . C(32) C(33) 1.585(17) yes . . C(2) H(2) 0.88(3) no . . C(4) H(3) 1.11(5) no . . C(4) H(4) 1.00(4) no . . C(4) H(5) 1.26(6) no . . C(5) H(6) 1.00(4) no . . C(5) H(7) 0.88(4) no . . C(5) H(8) 1.08(4) no . . C(7) H(9) 0.92(3) no . . C(9) H(10) 1.19(7) no . . C(9) H(11) 0.87(4) no . . C(9) H(12) 1.01(4) no . . C(10) H(13) 1.01(3) no . . C(10) H(14) 0.95(4) no . . C(10) H(15) 1.00(4) no . . C(12) H(16) 0.89(3) no . . C(14) H(17) 0.90(4) no . . C(14) H(18) 1.06(4) no . . C(14) H(19) 0.73(4) no . . C(15) H(20) 0.78(4) no . . C(15) H(21) 1.07(4) no . . C(15) H(22) 1.00(4) no . . C(18) H(23) 0.92(3) no . . C(19) H(24) 0.96(4) no . . C(20) H(25) 0.97(4) no . . C(21) H(26) 0.98(3) no . . C(23) H(27) 0.89(5) no . . C(23) H(28) 0.98(5) no . . C(23) H(29) 0.99(6) no . . C(24) H(30) 0.950 no . . C(24) H(31) 0.950 no . . C(25) H(32) 0.950 no . . C(25) H(33) 0.950 no . . C(26) H(34) 0.950 no . . C(26) H(35) 0.950 no . . C(27) H(36) 0.950 no . . C(27) H(37) 0.950 no . . B(1) H(1) 1.14(3) 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 S(1) Rh(1) S(2) 88.16(3) yes . . . S(1) Rh(1) N(2) 178.76(7) yes . . . S(1) Rh(1) N(4) 92.49(7) yes . . . S(1) Rh(1) N(6) 92.10(7) yes . . . S(1) Rh(1) N(7) 90.63(7) yes . . . S(2) Rh(1) N(2) 92.54(7) yes . . . S(2) Rh(1) N(4) 178.08(7) yes . . . S(2) Rh(1) N(6) 92.52(7) yes . . . S(2) Rh(1) N(7) 87.81(7) yes . . . N(2) Rh(1) N(4) 86.77(9) yes . . . N(2) Rh(1) N(6) 88.89(9) yes . . . N(2) Rh(1) N(7) 88.38(10) yes . . . N(4) Rh(1) N(6) 89.26(10) yes . . . N(4) Rh(1) N(7) 90.38(10) yes . . . N(6) Rh(1) N(7) 177.26(10) yes . . . Rh(1) S(1) C(16) 102.47(10) yes . . . Rh(1) S(2) C(17) 102.76(10) yes . . . C(24) O(1) C(27) 111.8(4) yes . . . C(28) O(2) C(31) 108.1(7) yes . . . C(28) O(3) C(33) 108.7(6) yes . . . N(2) N(1) C(3) 109.2(2) yes . . . N(2) N(1) B(1) 119.5(2) yes . . . C(3) N(1) B(1) 131.3(2) yes . . . Rh(1) N(2) N(1) 116.07(17) yes . . . Rh(1) N(2) C(1) 136.8(2) yes . . . N(1) N(2) C(1) 107.1(2) yes . . . N(4) N(3) C(8) 109.6(2) yes . . . N(4) N(3) B(1) 119.6(2) yes . . . C(8) N(3) B(1) 130.5(2) yes . . . Rh(1) N(4) N(3) 116.89(18) yes . . . Rh(1) N(4) C(6) 135.7(2) yes . . . N(3) N(4) C(6) 107.2(2) yes . . . N(6) N(5) C(13) 109.7(2) yes . . . N(6) N(5) B(1) 121.4(2) yes . . . C(13) N(5) B(1) 128.7(2) yes . . . Rh(1) N(6) N(5) 116.19(17) yes . . . Rh(1) N(6) C(11) 136.3(2) yes . . . N(5) N(6) C(11) 107.1(2) yes . . . Rh(1) N(7) C(22) 172.6(2) yes . . . N(2) C(1) C(2) 109.4(2) yes . . . N(2) C(1) C(4) 123.1(2) yes . . . C(2) C(1) C(4) 127.4(3) yes . . . C(1) C(2) C(3) 106.9(3) yes . . . N(1) C(3) C(2) 107.4(2) yes . . . N(1) C(3) C(5) 122.9(3) yes . . . C(2) C(3) C(5) 129.6(3) yes . . . N(4) C(6) C(7) 109.3(2) yes . . . N(4) C(6) C(9) 123.2(3) yes . . . C(7) C(6) C(9) 127.5(3) yes . . . C(6) C(7) C(8) 106.7(2) yes . . . N(3) C(8) C(7) 107.1(2) yes . . . N(3) C(8) C(10) 122.7(2) yes . . . C(7) C(8) C(10) 130.1(3) yes . . . N(6) C(11) C(12) 108.6(2) yes . . . N(6) C(11) C(14) 125.5(2) yes . . . C(12) C(11) C(14) 126.0(2) yes . . . C(11) C(12) C(13) 107.1(2) yes . . . N(5) C(13) C(12) 107.5(2) yes . . . N(5) C(13) C(15) 123.2(3) yes . . . C(12) C(13) C(15) 129.3(3) yes . . . S(1) C(16) C(17) 121.2(2) yes . . . S(1) C(16) C(21) 119.6(2) yes . . . C(17) C(16) C(21) 119.2(3) yes . . . S(2) C(17) C(16) 120.9(2) yes . . . S(2) C(17) C(18) 119.9(2) yes . . . C(16) C(17) C(18) 119.1(2) yes . . . C(17) C(18) C(19) 121.0(3) yes . . . C(18) C(19) C(20) 119.8(3) yes . . . C(19) C(20) C(21) 120.0(3) yes . . . C(16) C(21) C(20) 120.9(3) yes . . . N(7) C(22) C(23) 177.2(3) yes . . . O(1) C(24) C(25) 103.4(4) yes . . . C(24) C(25) C(26) 105.8(5) yes . . . C(25) C(26) C(27) 101.3(5) yes . . . O(1) C(27) C(26) 103.4(5) yes . . . O(2) C(28) C(29) 107.8(5) yes . . . O(3) C(28) C(29) 102.5(4) yes . . . C(28) C(29) C(30) 104.7(5) yes . . . C(28) C(29) C(32) 100.2(5) yes . . . C(29) C(30) C(31) 104.7(7) yes . . . O(2) C(31) C(30) 102.8(8) yes . . . C(29) C(32) C(33) 94.1(8) yes . . . O(3) C(33) C(32) 106.9(8) yes . . . N(1) B(1) N(3) 108.9(2) yes . . . N(1) B(1) N(5) 107.7(2) yes . . . N(3) B(1) N(5) 109.7(2) yes . . . C(1) C(2) H(2) 125(2) no . . . C(3) C(2) H(2) 128(2) no . . . C(1) C(4) H(3) 114(2) no . . . C(1) C(4) H(4) 105(2) no . . . C(1) C(4) H(5) 118(2) no . . . H(3) C(4) H(4) 118(3) no . . . H(3) C(4) H(5) 104(3) no . . . H(4) C(4) H(5) 97(3) no . . . C(3) C(5) H(6) 119(2) no . . . C(3) C(5) H(7) 112(2) no . . . C(3) C(5) H(8) 110(2) no . . . H(6) C(5) H(7) 108(3) no . . . H(6) C(5) H(8) 100(3) no . . . H(7) C(5) H(8) 106(3) no . . . C(6) C(7) H(9) 129(2) no . . . C(8) C(7) H(9) 125(2) no . . . C(6) C(9) H(10) 113(3) no . . . C(6) C(9) H(11) 103(2) no . . . C(6) C(9) H(12) 112(2) no . . . H(10) C(9) H(11) 122(4) no . . . H(10) C(9) H(12) 101(4) no . . . H(11) C(9) H(12) 105(3) no . . . C(8) C(10) H(13) 114(2) no . . . C(8) C(10) H(14) 108(2) no . . . C(8) C(10) H(15) 117(2) no . . . H(13) C(10) H(14) 106(3) no . . . H(13) C(10) H(15) 113(3) no . . . H(14) C(10) H(15) 98(3) no . . . C(11) C(12) H(16) 130(2) no . . . C(13) C(12) H(16) 123(2) no . . . C(11) C(14) H(17) 110(2) no . . . C(11) C(14) H(18) 109(2) no . . . C(11) C(14) H(19) 100(3) no . . . H(17) C(14) H(18) 112(3) no . . . H(17) C(14) H(19) 119(4) no . . . H(18) C(14) H(19) 107(4) no . . . C(13) C(15) H(20) 106(3) no . . . C(13) C(15) H(21) 108(2) no . . . C(13) C(15) H(22) 106(2) no . . . H(20) C(15) H(21) 111(4) no . . . H(20) C(15) H(22) 120(4) no . . . H(21) C(15) H(22) 105(3) no . . . C(17) C(18) H(23) 116(2) no . . . C(19) C(18) H(23) 123(2) no . . . C(18) C(19) H(24) 119(2) no . . . C(20) C(19) H(24) 121(2) no . . . C(19) C(20) H(25) 122(2) no . . . C(21) C(20) H(25) 118(2) no . . . C(16) C(21) H(26) 120(2) no . . . C(20) C(21) H(26) 119(2) no . . . C(22) C(23) H(27) 103(3) no . . . C(22) C(23) H(28) 105(3) no . . . C(22) C(23) H(29) 110(3) no . . . H(27) C(23) H(28) 115(4) no . . . H(27) C(23) H(29) 105(4) no . . . H(28) C(23) H(29) 117(4) no . . . O(1) C(24) H(30) 110.9 no . . . O(1) C(24) H(31) 111.1 no . . . C(25) C(24) H(30) 111.1 no . . . C(25) C(24) H(31) 110.9 no . . . H(30) C(24) H(31) 109.5 no . . . C(24) C(25) H(32) 110.2 no . . . C(24) C(25) H(33) 110.3 no . . . C(26) C(25) H(32) 109.7 no . . . C(26) C(25) H(33) 111.2 no . . . H(32) C(25) H(33) 109.5 no . . . C(25) C(26) H(34) 112.5 no . . . C(25) C(26) H(35) 110.7 no . . . C(27) C(26) H(34) 110.3 no . . . C(27) C(26) H(35) 112.4 no . . . H(34) C(26) H(35) 109.5 no . . . O(1) C(27) H(36) 109.6 no . . . O(1) C(27) H(37) 113.1 no . . . C(26) C(27) H(36) 109.5 no . . . C(26) C(27) H(37) 111.6 no . . . H(36) C(27) H(37) 109.5 no . . . N(1) B(1) H(1) 109.0(16) no . . . N(3) B(1) H(1) 110.7(16) no . . . N(5) B(1) H(1) 110.8(16) no . . . #===END #============================================================================== data___[TpMe2Rh(S2C6H4)(MeCN)]_THF _database_code_depnum_ccdc_archive 'CCDC 753658' #TrackingRef 'CIF-TpsRh1.txt' _audit_creation_date 2009-08-09 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H37 B N7 O Rh S2 ' _chemical_formula_moiety 'C27 H37 B N7 O Rh S2 ' _chemical_formula_weight 653.47 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 10.248(2) _cell_length_b 19.925(4) _cell_length_c 15.443(3) _cell_angle_alpha 90 _cell_angle_beta 101.7510(7) _cell_angle_gamma 90 _cell_volume 3087.3(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8563 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352.00 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.835 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_ambient_temperature 293.1 _diffrn_reflns_number 24530 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9927 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9927 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 7041 _reflns_number_gt 5356 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1110 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 7041 _refine_ls_number_parameters 392 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 0.8000\s(Fo^2^) + 0.0800]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.14 _refine_diff_density_min -0.58 _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) ; B B 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; 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) ; #============================================================================== # 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 Rh(1) Rh 0.54674(2) 0.217130(10) 0.389890(10) 0.03430(6) Uani 1.00 1 d . . . S(1) S 0.32992(7) 0.23500(4) 0.40492(5) 0.0505(2) Uani 1.00 1 d . . . S(2) S 0.58743(9) 0.33029(4) 0.41510(6) 0.0538(2) Uani 1.00 1 d . . . O(1) O 0.6183(7) 0.0576(6) 0.1377(5) 0.236(4) Uani 1.00 1 d . . . N(1) N 0.8058(2) 0.14350(11) 0.4139(2) 0.0391(6) Uani 1.00 1 d . . . N(2) N 0.7454(2) 0.20046(12) 0.3748(2) 0.0383(6) Uani 1.00 1 d . . . N(3) N 0.6042(2) 0.07055(12) 0.4101(2) 0.0403(6) Uani 1.00 1 d . . . N(4) N 0.5111(2) 0.11392(11) 0.3652(2) 0.0393(6) Uani 1.00 1 d . . . N(5) N 0.6952(2) 0.14215(11) 0.5416(1) 0.0393(6) Uani 1.00 1 d . . . N(6) N 0.6068(2) 0.19512(12) 0.5222(1) 0.0380(6) Uani 1.00 1 d . . . N(7) N 0.4964(3) 0.23335(13) 0.2582(2) 0.0470(7) Uani 1.00 1 d . . . C(1) C 0.8341(3) 0.2324(2) 0.3368(2) 0.0468(8) Uani 1.00 1 d . . . C(2) C 0.9533(3) 0.1959(2) 0.3527(2) 0.0511(9) Uani 1.00 1 d . . . C(3) C 0.9321(3) 0.1411(2) 0.4010(2) 0.0490(8) Uani 1.00 1 d . . . C(4) C 0.8060(4) 0.2949(2) 0.2846(3) 0.0709(13) Uani 1.00 1 d . . . C(5) C 1.0250(3) 0.0850(2) 0.4346(3) 0.081(1) Uani 1.00 1 d . . . C(6) C 0.4152(3) 0.0765(2) 0.3148(2) 0.0464(8) Uani 1.00 1 d . . . C(7) C 0.4486(3) 0.0091(2) 0.3280(2) 0.0546(9) Uani 1.00 1 d . . . C(8) C 0.5661(3) 0.0066(2) 0.3883(2) 0.0500(9) Uani 1.00 1 d . . . C(9) C 0.2952(3) 0.1054(2) 0.2539(2) 0.0650(10) Uani 1.00 1 d . . . C(10) C 0.6424(4) -0.0539(2) 0.4281(3) 0.0750(13) Uani 1.00 1 d . . . C(11) C 0.5940(3) 0.2225(1) 0.5993(2) 0.0442(8) Uani 1.00 1 d . . . C(12) C 0.6763(3) 0.1879(2) 0.6681(2) 0.0509(8) Uani 1.00 1 d . . . C(13) C 0.7379(3) 0.1389(2) 0.6307(2) 0.0471(8) Uani 1.00 1 d . . . C(14) C 0.5074(4) 0.2809(2) 0.6094(2) 0.0653(11) Uani 1.00 1 d . . . C(15) C 0.8415(3) 0.0899(2) 0.6737(2) 0.0668(11) Uani 1.00 1 d . . . C(16) C 0.3187(3) 0.3234(2) 0.4092(2) 0.0519(9) Uani 1.00 1 d . . . C(17) C 0.4297(4) 0.3643(2) 0.4148(2) 0.0573(10) Uani 1.00 1 d . . . C(18) C 0.4158(5) 0.4337(2) 0.4209(2) 0.0759(13) Uani 1.00 1 d . . . C(19) C 0.2929(6) 0.4623(3) 0.4202(3) 0.098(2) Uani 1.00 1 d . . . C(20) C 0.1815(6) 0.4217(3) 0.4121(3) 0.106(2) Uani 1.00 1 d . . . C(21) C 0.1938(4) 0.3529(2) 0.4079(3) 0.0796(13) Uani 1.00 1 d . . . C(22) C 0.4746(4) 0.2345(2) 0.1839(2) 0.0581(10) Uani 1.00 1 d . . . C(23) C 0.4487(5) 0.2351(3) 0.0873(3) 0.102(2) Uani 1.00 1 d . . . C(24) C 0.8536(9) 0.0605(5) 0.1800(6) 0.165(4) Uani 1.00 1 d . . . C(25) C 0.8089(9) -0.0007(5) 0.2105(6) 0.180(5) Uani 1.00 1 d . . . C(26) C 0.6813(10) -0.0114(4) 0.1583(7) 0.162(4) Uani 1.00 1 d . . . C(28) C 0.7370(12) 0.1016(4) 0.1607(5) 0.163(4) Uani 1.00 1 d . . . B(1) B 0.7310(3) 0.0983(2) 0.4688(2) 0.0394(8) Uani 1.00 1 d . . . H(1) H 0.791(3) 0.0584(13) 0.493(2) 0.033(7) Uiso 1.00 1 c . . . H(2) H 1.0328 0.2069 0.3332 0.062 Uiso 1.00 1 c R . . H(3) H 0.7730 0.2844 0.2241 0.090 Uiso 1.00 1 c R . . H(4) H 0.8862 0.3199 0.2903 0.090 Uiso 1.00 1 c R . . H(5) H 0.7416 0.3208 0.3063 0.090 Uiso 1.00 1 c R . . H(6) H 1.0730 0.0957 0.4923 0.098 Uiso 1.00 1 c R . . H(7) H 1.0858 0.0788 0.3963 0.098 Uiso 1.00 1 c R . . H(8) H 0.9755 0.0450 0.4367 0.098 Uiso 1.00 1 c R . . H(9) H 0.3984 -0.0281 0.3007 0.064 Uiso 1.00 1 c R . . H(10) H 0.2254 0.1099 0.2856 0.075 Uiso 1.00 1 c R . . H(11) H 0.2671 0.0764 0.2047 0.074 Uiso 1.00 1 c R . . H(12) H 0.3165 0.1482 0.2335 0.074 Uiso 1.00 1 c R . . H(13) H 0.7058 -0.0663 0.3938 0.088 Uiso 1.00 1 c R . . H(14) H 0.5823 -0.0901 0.4293 0.088 Uiso 1.00 1 c R . . H(15) H 0.6872 -0.0437 0.4867 0.088 Uiso 1.00 1 c R . . H(16) H 0.6868 0.1971 0.7295 0.061 Uiso 1.00 1 c R . . H(17) H 0.5570 0.3212 0.6091 0.079 Uiso 1.00 1 c R . . H(18) H 0.4778 0.2775 0.6637 0.079 Uiso 1.00 1 c R . . H(19) H 0.4326 0.2815 0.5616 0.079 Uiso 1.00 1 c R . . H(20) H 0.7999 0.0494 0.6864 0.078 Uiso 1.00 1 c R . . H(21) H 0.8904 0.1085 0.7272 0.078 Uiso 1.00 1 c R . . H(22) H 0.9003 0.0806 0.6350 0.077 Uiso 1.00 1 c R . . H(23) H 0.4927 0.4612 0.4258 0.091 Uiso 1.00 1 c R . . H(24) H 0.2848 0.5096 0.4250 0.116 Uiso 1.00 1 c R . . H(25) H 0.0963 0.4411 0.4102 0.123 Uiso 1.00 1 c R . . H(26) H 0.1184 0.3245 0.4043 0.093 Uiso 1.00 1 c R . . H(27) H 0.4520 0.2801 0.0674 0.122 Uiso 1.00 1 c R . . H(28) H 0.3631 0.2167 0.0643 0.122 Uiso 1.00 1 c R . . H(29) H 0.5146 0.2092 0.0673 0.122 Uiso 1.00 1 c R . . H(30) H 0.9221 0.0813 0.2220 0.208 Uiso 1.00 1 c R . . H(31) H 0.8852 0.0515 0.1274 0.208 Uiso 1.00 1 c R . . H(32) H 0.8685 -0.0367 0.2072 0.219 Uiso 1.00 1 c R . . H(33) H 0.8002 0.0051 0.2701 0.219 Uiso 1.00 1 c R . . H(34) H 0.6264 -0.0387 0.1865 0.202 Uiso 1.00 1 c R . . H(35) H 0.6919 -0.0321 0.1047 0.202 Uiso 1.00 1 c R . . H(36) H 0.7410 0.1303 0.1122 0.197 Uiso 1.00 1 c R . . H(37) H 0.7319 0.1279 0.2112 0.197 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 Rh(1) 0.03464(13) 0.03866(13) 0.02831(12) 0.00424(8) 0.00338(8) 0.00093(8) S(1) 0.0363(4) 0.0662(5) 0.0478(4) 0.0075(3) 0.0057(3) -0.0052(4) S(2) 0.0656(5) 0.0402(4) 0.0601(5) -0.0014(4) 0.0234(4) -0.0048(4) O(1) 0.165(6) 0.322(10) 0.243(8) 0.002(7) 0.091(5) 0.006(8) N(1) 0.0350(11) 0.0431(12) 0.0373(12) 0.0032(9) 0.0032(9) 0.0022(10) N(2) 0.0346(11) 0.0437(13) 0.0371(12) 0.0046(9) 0.0087(9) 0.0028(10) N(3) 0.0378(12) 0.0411(12) 0.0386(12) 0.0000(10) -0.0004(10) 0.0020(10) N(4) 0.0391(11) 0.0388(12) 0.0363(12) -0.0010(10) -0.0008(9) -0.0011(10) N(5) 0.0388(11) 0.0439(13) 0.0319(11) -0.0027(10) -0.0008(9) 0.0065(9) N(6) 0.0386(11) 0.0454(12) 0.0278(11) 0.0012(10) 0.0017(9) 0.0006(9) N(7) 0.052(1) 0.052(1) 0.0347(13) 0.0126(11) 0.0045(11) 0.0062(11) C(1) 0.048(2) 0.050(2) 0.046(2) -0.0038(13) 0.0163(13) 0.0032(13) C(2) 0.038(1) 0.064(2) 0.054(2) -0.002(1) 0.0161(13) -0.001(2) C(3) 0.035(1) 0.062(2) 0.049(2) 0.0089(13) 0.0059(12) 0.002(1) C(4) 0.078(3) 0.064(2) 0.082(3) 0.002(2) 0.044(2) 0.015(2) C(5) 0.046(2) 0.095(3) 0.104(3) 0.028(2) 0.018(2) 0.032(3) C(6) 0.041(1) 0.052(2) 0.043(2) -0.0062(13) 0.0032(12) -0.0079(13) C(7) 0.053(2) 0.048(2) 0.060(2) -0.013(1) 0.006(2) -0.007(2) C(8) 0.056(2) 0.039(2) 0.054(2) -0.0028(13) 0.010(2) -0.0021(13) C(9) 0.054(2) 0.070(2) 0.061(2) -0.006(2) -0.012(2) -0.010(2) C(10) 0.078(3) 0.046(2) 0.095(3) 0.004(2) 0.004(2) 0.004(2) C(11) 0.044(2) 0.057(2) 0.0310(13) -0.0040(13) 0.0068(12) -0.0025(12) C(12) 0.057(2) 0.067(2) 0.0266(13) -0.008(2) 0.0052(12) -0.0003(13) C(13) 0.045(2) 0.057(2) 0.035(1) -0.0104(13) -0.0025(12) 0.0089(13) C(14) 0.081(3) 0.079(3) 0.038(2) 0.007(2) 0.016(2) -0.012(2) C(15) 0.062(2) 0.081(3) 0.050(2) 0.003(2) -0.008(2) 0.019(2) C(16) 0.054(2) 0.067(2) 0.032(1) 0.024(2) 0.0025(13) -0.006(1) C(17) 0.086(2) 0.054(2) 0.032(1) 0.024(2) 0.010(2) 0.0023(13) C(18) 0.124(4) 0.052(2) 0.053(2) 0.027(2) 0.021(2) 0.002(2) C(19) 0.152(5) 0.080(3) 0.059(3) 0.063(3) 0.014(3) -0.003(2) C(20) 0.111(4) 0.132(5) 0.064(3) 0.085(4) -0.009(3) -0.017(3) C(21) 0.069(2) 0.105(3) 0.058(2) 0.040(2) -0.003(2) -0.016(2) C(22) 0.072(2) 0.063(2) 0.038(2) 0.023(2) 0.010(2) 0.007(2) C(23) 0.139(5) 0.127(4) 0.038(2) 0.056(4) 0.012(2) 0.011(2) C(24) 0.173(8) 0.152(7) 0.196(9) -0.047(6) 0.101(7) -0.074(6) C(25) 0.147(7) 0.177(9) 0.224(11) 0.015(7) 0.055(7) 0.012(8) C(26) 0.154(7) 0.099(5) 0.252(11) -0.018(5) 0.083(7) -0.028(6) C(28) 0.232(10) 0.128(6) 0.133(6) -0.035(7) 0.046(7) -0.044(5) B(1) 0.038(2) 0.040(2) 0.036(2) 0.0033(13) 0.0002(12) 0.0051(13) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _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 Rh(1) S(1) 2.3082(8) ? . . Rh(1) S(2) 2.3115(8) ? . . Rh(1) N(2) 2.122(2) ? . . Rh(1) N(4) 2.110(2) ? . . Rh(1) N(6) 2.058(2) ? . . Rh(1) N(7) 2.019(2) ? . . S(1) C(16) 1.766(4) ? . . S(2) C(17) 1.752(4) ? . . O(1) C(26) 1.52(1) ? . . O(1) C(28) 1.48(1) ? . . N(1) N(2) 1.373(3) ? . . N(1) C(3) 1.350(4) ? . . N(1) B(1) 1.543(4) ? . . N(2) C(1) 1.339(4) ? . . N(3) N(4) 1.367(3) ? . . N(3) C(8) 1.354(4) ? . . N(3) B(1) 1.528(4) ? . . N(4) C(6) 1.347(3) ? . . N(5) N(6) 1.383(3) ? . . N(5) C(13) 1.357(3) ? . . N(5) B(1) 1.527(4) ? . . N(6) C(11) 1.340(4) ? . . N(7) C(22) 1.125(4) ? . . C(1) C(2) 1.401(4) ? . . C(1) C(4) 1.479(5) ? . . C(2) C(3) 1.365(5) ? . . C(3) C(5) 1.490(5) ? . . C(6) C(7) 1.391(4) ? . . C(6) C(9) 1.503(4) ? . . C(7) C(8) 1.365(4) ? . . C(8) C(10) 1.500(5) ? . . C(10) C(8) 1.500(5) ? . . C(11) C(12) 1.396(4) ? . . C(11) C(14) 1.491(5) ? . . C(12) C(13) 1.354(5) ? . . C(13) C(15) 1.496(5) ? . . C(16) C(17) 1.389(5) ? . . C(16) C(21) 1.404(5) ? . . C(17) C(18) 1.394(5) ? . . C(18) C(19) 1.381(8) ? . . C(19) C(20) 1.384(8) ? . . C(20) C(21) 1.379(8) ? . . C(22) C(23) 1.461(5) ? . . C(24) C(25) 1.42(1) ? . . C(24) C(28) 1.43(1) ? . . C(25) C(26) 1.41(1) ? . . C(2) H(2) 0.9500 ? . . C(4) H(3) 0.9500 ? . . C(4) H(4) 0.9499 ? . . C(4) H(5) 0.9499 ? . . C(5) H(6) 0.9500 ? . . C(5) H(7) 0.9499 ? . . C(5) H(8) 0.9500 ? . . C(7) H(9) 0.9500 ? . . C(9) H(10) 0.9500 ? . . C(9) H(11) 0.9500 ? . . C(9) H(12) 0.9500 ? . . C(10) H(13) 0.9499 ? . . C(10) H(14) 0.9499 ? . . C(10) H(15) 0.9500 ? . . C(12) H(16) 0.9500 ? . . C(14) H(17) 0.9500 ? . . C(14) H(18) 0.9500 ? . . C(14) H(19) 0.9500 ? . . C(15) H(20) 0.9499 ? . . C(15) H(21) 0.9500 ? . . C(15) H(22) 0.9500 ? . . C(18) H(23) 0.9500 ? . . C(19) H(24) 0.9501 ? . . C(20) H(25) 0.9500 ? . . C(21) H(26) 0.9500 ? . . C(23) H(27) 0.9500 ? . . C(23) H(28) 0.9501 ? . . C(23) H(29) 0.9501 ? . . C(24) H(30) 0.9499 ? . . C(24) H(31) 0.9500 ? . . C(25) H(32) 0.9500 ? . . C(25) H(33) 0.9501 ? . . C(26) H(34) 0.9500 ? . . C(26) H(35) 0.9501 ? . . C(28) H(36) 0.9500 ? . . C(28) H(37) 0.9499 ? . . B(1) H(1) 1.03(3) ? . . H(13) C(10) 0.9499 ? . . H(14) C(10) 0.9499 ? . . H(15) C(10) 0.9500 ? . . H(32) C(25) 0.9500 ? . . 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 S(2) Rh(1) S(1) 88.68(3) ? . . . N(2) Rh(1) S(1) 179.45(6) ? . . . N(4) Rh(1) S(1) 91.93(7) ? . . . N(6) Rh(1) S(1) 91.86(7) ? . . . N(7) Rh(1) S(1) 91.30(8) ? . . . Rh(1) S(1) C(16) 103.2(1) ? . . . N(2) Rh(1) S(2) 91.55(7) ? . . . N(4) Rh(1) S(2) 179.10(7) ? . . . N(6) Rh(1) S(2) 91.91(7) ? . . . N(7) Rh(1) S(2) 90.79(8) ? . . . Rh(1) S(2) C(17) 104.0(1) ? . . . Rh(1) N(2) N(1) 116.0(2) ? . . . N(4) Rh(1) N(2) 87.83(9) ? . . . N(6) Rh(1) N(2) 88.63(9) ? . . . N(7) Rh(1) N(2) 88.2(1) ? . . . Rh(1) N(2) C(1) 136.5(2) ? . . . Rh(1) N(4) N(3) 116.6(2) ? . . . N(6) Rh(1) N(4) 88.73(9) ? . . . N(7) Rh(1) N(4) 88.5(1) ? . . . Rh(1) N(4) C(6) 136.3(2) ? . . . Rh(1) N(6) N(5) 115.3(2) ? . . . N(7) Rh(1) N(6) 175.9(1) ? . . . Rh(1) N(6) C(11) 137.0(2) ? . . . Rh(1) N(7) C(22) 171.2(3) ? . . . S(1) C(16) C(17) 121.9(3) ? . . . S(1) C(16) C(21) 118.9(3) ? . . . S(2) C(17) C(16) 121.1(3) ? . . . S(2) C(17) C(18) 119.3(3) ? . . . O(1) C(26) C(25) 106.8(7) ? . . . C(28) O(1) C(26) 101.0(6) ? . . . O(1) C(28) C(24) 108.7(7) ? . . . N(1) N(2) C(1) 107.5(2) ? . . . B(1) N(1) N(2) 119.6(2) ? . . . C(3) N(1) N(2) 109.0(2) ? . . . B(1) N(1) C(3) 131.2(2) ? . . . N(1) C(3) C(2) 108.4(3) ? . . . N(1) C(3) C(5) 122.7(3) ? . . . N(1) B(1) N(3) 110.1(2) ? . . . N(1) B(1) N(5) 107.0(2) ? . . . N(2) C(1) C(4) 124.4(3) ? . . . N(2) C(1) C(2) 108.8(3) ? . . . N(3) N(4) C(6) 107.2(2) ? . . . B(1) N(3) N(4) 119.5(2) ? . . . C(8) N(3) N(4) 109.4(2) ? . . . B(1) N(3) C(8) 131.0(2) ? . . . N(3) C(8) C(7) 107.8(3) ? . . . N(3) C(8) C(10) 123.7(3) ? . . . N(3) B(1) N(5) 109.9(2) ? . . . N(4) C(6) C(9) 123.9(3) ? . . . N(4) C(6) C(7) 108.7(2) ? . . . N(5) N(6) C(11) 107.3(2) ? . . . B(1) N(5) N(6) 121.5(2) ? . . . C(13) N(5) N(6) 108.5(2) ? . . . B(1) N(5) C(13) 130.0(2) ? . . . N(5) C(13) C(12) 108.4(2) ? . . . N(5) C(13) C(15) 122.3(3) ? . . . N(6) C(11) C(14) 125.4(3) ? . . . N(6) C(11) C(12) 108.8(3) ? . . . N(7) C(22) C(23) 178.8(4) ? . . . C(4) C(1) C(2) 126.8(3) ? . . . C(1) C(2) C(3) 106.3(3) ? . . . C(2) C(3) C(5) 128.9(3) ? . . . C(9) C(6) C(7) 127.3(3) ? . . . C(6) C(7) C(8) 106.9(3) ? . . . C(7) C(8) C(10) 128.5(3) ? . . . C(14) C(11) C(12) 125.9(3) ? . . . C(11) C(12) C(13) 107.0(3) ? . . . C(12) C(13) C(15) 129.2(3) ? . . . C(21) C(16) C(17) 119.2(3) ? . . . C(16) C(17) C(18) 119.5(4) ? . . . C(16) C(21) C(20) 120.5(4) ? . . . C(17) C(18) C(19) 120.9(4) ? . . . C(18) C(19) C(20) 119.5(5) ? . . . C(19) C(20) C(21) 120.3(5) ? . . . C(24) C(25) C(26) 105.4(8) ? . . . C(28) C(24) C(25) 104.5(8) ? . . . O(1) C(26) H(34) 110.2787 ? . . . O(1) C(26) H(35) 109.2145 ? . . . O(1) C(28) H(36) 109.4750 ? . . . O(1) C(28) H(37) 110.0836 ? . . . N(1) B(1) H(1) 109(1) ? . . . N(3) B(1) H(1) 107(1) ? . . . N(5) B(1) H(1) 112(1) ? . . . C(1) C(2) H(2) 126.7815 ? . . . C(1) C(4) H(5) 109.7090 ? . . . C(1) C(4) H(3) 109.9053 ? . . . C(1) C(4) H(4) 108.7925 ? . . . H(2) C(2) C(3) 126.8830 ? . . . C(3) C(5) H(6) 109.3419 ? . . . C(3) C(5) H(7) 109.6178 ? . . . C(3) C(5) H(8) 109.4516 ? . . . H(5) C(4) H(3) 109.4704 ? . . . H(4) C(4) H(3) 109.4725 ? . . . H(5) C(4) H(4) 109.4754 ? . . . H(7) C(5) H(6) 109.4697 ? . . . H(8) C(5) H(6) 109.4750 ? . . . H(8) C(5) H(7) 109.4713 ? . . . C(6) C(7) H(9) 126.4799 ? . . . C(6) C(9) H(12) 109.6586 ? . . . C(6) C(9) H(10) 108.6223 ? . . . C(6) C(9) H(11) 110.1183 ? . . . H(9) C(7) C(8) 126.6182 ? . . . C(8) C(10) H(13) 109.8947 ? . . . C(8) C(10) H(14) 109.3821 ? . . . C(8) C(10) H(15) 109.1359 ? . . . H(12) C(9) H(10) 109.4761 ? . . . H(11) C(9) H(10) 109.4717 ? . . . H(12) C(9) H(11) 109.4766 ? . . . H(14) C(10) H(13) 109.4766 ? . . . H(15) C(10) H(13) 109.4699 ? . . . H(15) C(10) H(14) 109.4670 ? . . . C(11) C(12) H(16) 126.3064 ? . . . C(11) C(14) H(19) 109.4165 ? . . . C(11) C(14) H(17) 109.1726 ? . . . C(11) C(14) H(18) 109.8158 ? . . . H(16) C(12) C(13) 126.6696 ? . . . C(13) C(15) H(22) 109.3289 ? . . . C(13) C(15) H(20) 109.7148 ? . . . C(13) C(15) H(21) 109.3680 ? . . . H(19) C(14) H(17) 109.4736 ? . . . H(18) C(14) H(17) 109.4732 ? . . . H(19) C(14) H(18) 109.4749 ? . . . H(22) C(15) H(20) 109.4751 ? . . . H(21) C(15) H(20) 109.4747 ? . . . H(22) C(15) H(21) 109.4655 ? . . . C(16) C(21) H(26) 118.6486 ? . . . C(17) C(18) H(23) 118.8501 ? . . . H(23) C(18) C(19) 120.2024 ? . . . C(18) C(19) H(24) 120.1837 ? . . . C(19) C(20) H(25) 120.0415 ? . . . H(24) C(19) C(20) 120.2745 ? . . . C(20) C(21) H(26) 120.8684 ? . . . H(25) C(20) C(21) 119.6748 ? . . . C(22) C(23) H(29) 109.4771 ? . . . C(22) C(23) H(27) 109.0663 ? . . . C(22) C(23) H(28) 109.8611 ? . . . H(29) C(23) H(27) 109.4804 ? . . . H(28) C(23) H(27) 109.4760 ? . . . H(29) C(23) H(28) 109.4656 ? . . . H(30) C(24) C(25) 113.1057 ? . . . H(31) C(24) C(25) 108.2635 ? . . . C(24) C(25) H(32) 112.1248 ? . . . C(24) C(25) H(33) 108.6168 ? . . . H(30) C(24) C(28) 111.2101 ? . . . H(31) C(24) C(28) 110.2144 ? . . . C(24) C(28) H(36) 109.9311 ? . . . C(24) C(28) H(37) 109.1536 ? . . . H(31) C(24) H(30) 109.4587 ? . . . H(32) C(25) C(26) 112.7784 ? . . . H(33) C(25) C(26) 108.3125 ? . . . C(25) C(26) H(34) 113.1066 ? . . . C(25) C(26) H(35) 107.9193 ? . . . H(33) C(25) H(32) 109.4625 ? . . . H(35) C(26) H(34) 109.4619 ? . . . H(37) C(28) H(36) 109.4620 ? . . . #===END #============================================================================== data___[TpMe2RhI2(MeCN)]-THF _database_code_depnum_ccdc_archive 'CCDC 753659' #TrackingRef 'CIF-TpsRh1.txt' _audit_creation_date 2009-08-09 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C21 H33 B I2 N7 O Rh ' _chemical_formula_moiety 'C21 H33 B I2 N7 O Rh ' _chemical_formula_weight 767.06 _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 7.9782(15) _cell_length_b 13.431(3) _cell_length_c 26.285(5) _cell_angle_alpha 90.0000 _cell_angle_beta 97.916(3) _cell_angle_gamma 90.0000 _cell_volume 2789.8(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8328 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488.00 _exptl_absorpt_coefficient_mu 2.851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.439 _exptl_absorpt_correction_T_max 0.652 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_ambient_temperature 113.1 _diffrn_reflns_number 33333 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_theta_max 27.87 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 #============================================================================== # 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 6664 _reflns_number_gt 5803 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.1166 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 6665 _refine_ls_number_parameters 361 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0011Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0019 _refine_diff_density_max 1.35 _refine_diff_density_min -0.92 _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) ; B B 0.001 0.001 ; 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) ; 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) ; #============================================================================== # 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 0.83277(4) 0.53564(3) 0.259160(10) 0.01855(8) Uani 1.00 1 d . . . I(2) I 0.79053(4) 0.33399(2) 0.155690(10) 0.01881(8) Uani 1.00 1 d . . . Rh(1) Rh 0.62380(4) 0.50027(3) 0.172440(10) 0.01134(8) Uani 1.00 1 d . . . O(1) O 0.872(2) 0.1051(14) 0.0227(7) 0.102(6) Uani 0.50 1 d P . . O(2) O 0.6743(13) -0.0034(8) 0.1028(4) 0.054(3) Uani 0.50 1 d P . . N(1) N 0.4238(4) 0.5590(3) 0.07413(14) 0.0152(9) Uani 1.00 1 d . . . N(2) N 0.4532(4) 0.4784(2) 0.10614(15) 0.0140(8) Uani 1.00 1 d . . . N(3) N 0.4477(4) 0.6900(2) 0.14295(14) 0.0140(8) Uani 1.00 1 d . . . N(4) N 0.4835(4) 0.6265(2) 0.18387(14) 0.0141(8) Uani 1.00 1 d . . . N(5) N 0.6939(4) 0.6522(3) 0.09810(15) 0.0158(9) Uani 1.00 1 d . . . N(6) N 0.7745(4) 0.5819(3) 0.13056(14) 0.0155(9) Uani 1.00 1 d . . . N(7) N 0.4695(4) 0.4222(3) 0.21218(15) 0.0167(9) Uani 1.00 1 d . . . C(1) C 0.3536(5) 0.4035(4) 0.08596(18) 0.0193(11) Uani 1.00 1 d . . . C(2) C 0.2612(6) 0.4365(4) 0.03948(19) 0.0222(12) Uani 1.00 1 d . . . C(3) C 0.3093(5) 0.5337(4) 0.03303(18) 0.0200(11) Uani 1.00 1 d . . . C(4) C 0.3361(6) 0.3041(4) 0.1102(2) 0.0276(13) Uani 1.00 1 d . . . C(5) C 0.2548(6) 0.6032(4) -0.01025(19) 0.0279(13) Uani 1.00 1 d . . . C(6) C 0.4051(5) 0.6634(3) 0.22256(18) 0.0162(10) Uani 1.00 1 d . . . C(7) C 0.3230(5) 0.7515(3) 0.20574(18) 0.0190(11) Uani 1.00 1 d . . . C(8) C 0.3517(5) 0.7667(3) 0.15609(18) 0.0176(11) Uani 1.00 1 d . . . C(9) C 0.4041(6) 0.6147(4) 0.27349(18) 0.0240(12) Uani 1.00 1 d . . . C(10) C 0.3005(6) 0.8529(3) 0.1209(2) 0.0245(12) Uani 1.00 1 d . . . C(11) C 0.9418(5) 0.5907(3) 0.12724(18) 0.0179(11) Uani 1.00 1 d . . . C(12) C 0.9638(6) 0.6646(3) 0.09215(19) 0.0204(11) Uani 1.00 1 d . . . C(13) C 0.8082(6) 0.7028(3) 0.07450(18) 0.0188(11) Uani 1.00 1 d . . . C(14) C 1.0799(6) 0.5291(4) 0.1552(2) 0.0290(14) Uani 1.00 1 d . . . C(15) C 0.7591(7) 0.7854(4) 0.0376(2) 0.0302(14) Uani 1.00 1 d . . . C(16) C 0.3766(6) 0.3832(3) 0.23409(19) 0.0206(11) Uani 1.00 1 d . . . C(17) C 0.2548(6) 0.3345(4) 0.2622(2) 0.0310(14) Uani 1.00 1 d . . . C(18) C 0.974(3) 0.104(2) 0.0695(11) 0.093(9) Uani 0.50 1 d P . . C(19) C 0.8571(14) 0.0384(12) 0.1088(5) 0.115(5) Uani 1.00 1 d . . . C(20) C 0.682(2) 0.070(2) 0.0759(7) 0.065(6) Uani 0.50 1 d P . . C(21) C 0.717(3) 0.0787(18) 0.0212(9) 0.075(8) Uani 0.50 1 d P . . C(22) C 0.894(5) 0.074(2) 0.0675(12) 0.130(13) Uani 0.50 1 d P . . C(23) C 0.678(3) 0.110(2) 0.0431(13) 0.090(10) Uani 0.50 1 d P . . C(24) C 0.589(3) 0.072(2) 0.0773(11) 0.092(9) Uani 0.50 1 d P . . B(1) B 0.5009(6) 0.6607(3) 0.0906(2) 0.0147(11) Uani 1.00 1 d . . . H(1) H 0.473(6) 0.713(4) 0.063(2) 0.0184 Uiso 1.00 1 c . . . H(2) H 0.1815 0.3990 0.0171 0.026 Uiso 1.00 1 c R . . H(3) H 0.4174 0.2594 0.0999 0.033 Uiso 1.00 1 c R . . H(4) H 0.2256 0.2786 0.0998 0.033 Uiso 1.00 1 c R . . H(5) H 0.3543 0.3112 0.1465 0.033 Uiso 1.00 1 c R . . H(6) H 0.1594 0.6403 -0.0031 0.033 Uiso 1.00 1 c R . . H(7) H 0.2255 0.5663 -0.0410 0.033 Uiso 1.00 1 c R . . H(8) H 0.3450 0.6474 -0.0142 0.033 Uiso 1.00 1 c R . . H(9) H 0.2586 0.7931 0.2250 0.023 Uiso 1.00 1 c R . . H(10) H 0.3090 0.5717 0.2719 0.029 Uiso 1.00 1 c R . . H(11) H 0.3972 0.6643 0.2989 0.029 Uiso 1.00 1 c R . . H(12) H 0.5050 0.5772 0.2821 0.029 Uiso 1.00 1 c R . . H(13) H 0.3835 0.9039 0.1264 0.029 Uiso 1.00 1 c R . . H(14) H 0.1945 0.8782 0.1276 0.030 Uiso 1.00 1 c R . . H(15) H 0.2909 0.8309 0.0863 0.029 Uiso 1.00 1 c R . . H(16) H 1.0683 0.6851 0.0821 0.025 Uiso 1.00 1 c R . . H(17) H 1.1199 0.5595 0.1872 0.035 Uiso 1.00 1 c R . . H(18) H 1.1700 0.5240 0.1352 0.035 Uiso 1.00 1 c R . . H(19) H 1.0380 0.4644 0.1611 0.035 Uiso 1.00 1 c R . . H(20) H 0.7354 0.7593 0.0038 0.037 Uiso 1.00 1 c R . . H(21) H 0.8499 0.8315 0.0391 0.037 Uiso 1.00 1 c R . . H(22) H 0.6615 0.8182 0.0464 0.037 Uiso 1.00 1 c R . . H(23) H 0.2836 0.3476 0.2979 0.039 Uiso 1.00 1 c R . . H(24) H 0.2571 0.2648 0.2564 0.039 Uiso 1.00 1 c R . . H(25) H 0.1445 0.3594 0.2509 0.039 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) 0.01631(16) 0.02430(18) 0.01396(16) 0.00016(12) -0.00178(11) -0.00118(11) I(2) 0.01954(17) 0.01810(16) 0.01957(17) 0.00209(11) 0.00552(12) 0.00098(11) Rh(1) 0.00957(17) 0.01431(18) 0.01016(17) -0.00017(12) 0.00146(12) -0.00026(12) O(1) 0.089(11) 0.110(14) 0.106(13) 0.004(10) 0.009(10) 0.007(11) O(2) 0.048(6) 0.040(5) 0.074(8) 0.004(4) 0.012(5) -0.012(5) N(1) 0.0122(17) 0.0203(19) 0.0129(17) -0.0009(14) 0.0006(13) -0.0019(15) N(2) 0.0120(17) 0.0155(18) 0.0142(17) -0.0005(14) 0.0006(14) -0.0006(14) N(3) 0.0116(17) 0.0151(18) 0.0146(17) 0.0011(14) -0.0003(13) 0.0003(14) N(4) 0.0143(17) 0.0159(18) 0.0122(17) -0.0002(14) 0.0019(13) -0.0027(14) N(5) 0.0153(18) 0.0181(19) 0.0143(18) 0.0004(14) 0.0029(14) 0.0011(14) N(6) 0.0131(17) 0.020(2) 0.0135(17) -0.0012(14) 0.0035(13) -0.0023(14) N(7) 0.0144(17) 0.020(2) 0.0158(18) 0.0034(15) 0.0026(14) 0.0020(15) C(1) 0.011(2) 0.028(2) 0.018(2) -0.0013(18) 0.0017(17) -0.0067(19) C(2) 0.018(2) 0.029(2) 0.018(2) -0.0015(19) -0.0014(18) -0.005(2) C(3) 0.013(2) 0.032(2) 0.015(2) 0.0020(19) 0.0024(17) -0.0032(19) C(4) 0.023(2) 0.030(2) 0.029(2) -0.006(2) 0.001(2) -0.008(2) C(5) 0.021(2) 0.047(3) 0.014(2) 0.000(2) -0.0046(18) 0.005(2) C(6) 0.013(2) 0.021(2) 0.015(2) -0.0006(17) 0.0028(16) -0.0039(17) C(7) 0.016(2) 0.021(2) 0.020(2) 0.0036(18) 0.0018(17) -0.0030(18) C(8) 0.015(2) 0.018(2) 0.019(2) 0.0024(17) 0.0005(17) -0.0057(18) C(9) 0.026(2) 0.031(2) 0.016(2) 0.005(2) 0.0072(19) -0.003(2) C(10) 0.026(2) 0.020(2) 0.027(2) 0.004(2) 0.003(2) 0.001(2) C(11) 0.013(2) 0.022(2) 0.019(2) -0.0026(17) 0.0022(16) -0.0040(18) C(12) 0.015(2) 0.028(2) 0.020(2) -0.0045(18) 0.0064(18) -0.0001(19) C(13) 0.020(2) 0.020(2) 0.018(2) -0.0047(18) 0.0077(18) -0.0009(18) C(14) 0.013(2) 0.040(3) 0.034(3) -0.003(2) 0.003(2) 0.002(2) C(15) 0.033(2) 0.027(2) 0.033(2) -0.007(2) 0.013(2) 0.002(2) C(16) 0.019(2) 0.023(2) 0.020(2) 0.0036(18) 0.0029(18) 0.0051(19) C(17) 0.025(2) 0.030(2) 0.042(3) 0.002(2) 0.017(2) 0.013(2) C(18) 0.069(14) 0.12(2) 0.089(18) -0.038(14) 0.012(12) -0.025(16) C(19) 0.062(6) 0.178(14) 0.093(8) 0.036(7) -0.034(6) -0.065(9) C(20) 0.054(11) 0.106(18) 0.038(9) 0.008(13) 0.018(9) 0.001(10) C(21) 0.103(19) 0.063(14) 0.064(14) 0.002(13) 0.030(13) 0.030(11) C(22) 0.20(3) 0.12(2) 0.10(2) -0.11(2) 0.11(2) -0.071(18) C(23) 0.082(19) 0.09(2) 0.09(2) -0.005(14) -0.004(16) -0.022(17) C(24) 0.059(13) 0.11(2) 0.10(2) -0.008(15) 0.000(14) 0.031(16) B(1) 0.014(2) 0.015(2) 0.015(2) -0.0031(18) 0.0018(18) 0.0005(18) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _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) 2.6747(3) yes . . I(2) Rh(1) 2.6669(4) yes . . Rh(1) N(2) 2.079(3) yes . . Rh(1) N(4) 2.076(3) yes . . Rh(1) N(6) 2.055(4) yes . . Rh(1) N(7) 2.015(4) yes . . O(1) C(18) 1.38(3) yes . . O(1) C(21) 1.28(3) yes . . O(2) C(19) 1.551(16) yes . . O(2) C(24) 1.35(3) yes . . N(1) N(2) 1.372(5) yes . . N(1) C(3) 1.358(5) yes . . N(1) B(1) 1.536(6) yes . . N(2) C(1) 1.345(6) yes . . N(3) N(4) 1.372(5) yes . . N(3) C(8) 1.356(6) yes . . N(3) B(1) 1.546(6) yes . . N(4) C(6) 1.359(6) yes . . N(5) N(6) 1.371(5) yes . . N(5) C(13) 1.355(6) yes . . N(5) B(1) 1.530(6) yes . . N(6) C(11) 1.355(5) yes . . N(7) C(16) 1.129(6) yes . . C(1) C(2) 1.409(6) yes . . C(1) C(4) 1.494(7) yes . . C(2) C(3) 1.377(7) yes . . C(3) C(5) 1.489(7) yes . . C(6) C(7) 1.395(6) yes . . C(6) C(9) 1.491(6) yes . . C(7) C(8) 1.371(6) yes . . C(8) C(10) 1.503(6) yes . . C(11) C(12) 1.383(7) yes . . C(11) C(14) 1.489(6) yes . . C(12) C(13) 1.364(6) yes . . C(13) C(15) 1.490(7) yes . . C(16) C(17) 1.455(8) yes . . C(18) C(19) 1.73(3) yes . . C(19) C(20) 1.60(2) yes . . C(19) C(22) 1.26(3) yes . . C(20) C(21) 1.51(3) yes . . C(22) C(23) 1.81(4) yes . . C(23) C(24) 1.32(4) yes . . C(2) 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(5) H(8) 0.950 no . . C(7) 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(10) H(13) 0.950 no . . C(10) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(12) H(16) 0.950 no . . C(14) H(17) 0.950 no . . C(14) H(18) 0.950 no . . C(14) H(19) 0.950 no . . C(15) H(20) 0.950 no . . C(15) H(21) 0.950 no . . C(15) H(22) 0.950 no . . C(17) H(23) 0.950 no . . C(17) H(24) 0.950 no . . C(17) H(25) 0.950 no . . B(1) H(1) 1.01(5) 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) 91.312(13) yes . . . I(1) Rh(1) N(2) 177.08(11) yes . . . I(1) Rh(1) N(4) 90.96(9) yes . . . I(1) Rh(1) N(6) 91.13(9) yes . . . I(1) Rh(1) N(7) 90.24(10) yes . . . I(2) Rh(1) N(2) 91.54(10) yes . . . I(2) Rh(1) N(4) 177.28(9) yes . . . I(2) Rh(1) N(6) 90.96(11) yes . . . I(2) Rh(1) N(7) 90.24(11) yes . . . N(2) Rh(1) N(4) 86.16(14) yes . . . N(2) Rh(1) N(6) 89.45(14) yes . . . N(2) Rh(1) N(7) 89.13(15) yes . . . N(4) Rh(1) N(6) 90.49(15) yes . . . N(4) Rh(1) N(7) 88.27(15) yes . . . N(6) Rh(1) N(7) 178.16(14) yes . . . C(18) O(1) C(21) 118(2) yes . . . C(19) O(2) C(24) 100.3(14) yes . . . N(2) N(1) C(3) 109.3(3) yes . . . N(2) N(1) B(1) 120.1(3) yes . . . C(3) N(1) B(1) 130.2(4) yes . . . Rh(1) N(2) N(1) 116.1(2) yes . . . Rh(1) N(2) C(1) 136.0(3) yes . . . N(1) N(2) C(1) 107.9(3) yes . . . N(4) N(3) C(8) 109.7(3) yes . . . N(4) N(3) B(1) 119.1(3) yes . . . C(8) N(3) B(1) 130.8(3) yes . . . Rh(1) N(4) N(3) 116.9(2) yes . . . Rh(1) N(4) C(6) 136.0(3) yes . . . N(3) N(4) C(6) 107.0(3) yes . . . N(6) N(5) C(13) 110.1(3) yes . . . N(6) N(5) B(1) 120.6(3) yes . . . C(13) N(5) B(1) 129.2(3) yes . . . Rh(1) N(6) N(5) 116.2(2) yes . . . Rh(1) N(6) C(11) 137.3(3) yes . . . N(5) N(6) C(11) 106.4(3) yes . . . Rh(1) N(7) C(16) 175.9(4) yes . . . N(2) C(1) C(2) 108.4(4) yes . . . N(2) C(1) C(4) 125.8(4) yes . . . C(2) C(1) C(4) 125.7(4) yes . . . C(1) C(2) C(3) 106.5(4) yes . . . N(1) C(3) C(2) 107.9(4) yes . . . N(1) C(3) C(5) 123.0(4) yes . . . C(2) C(3) C(5) 129.1(4) yes . . . N(4) C(6) C(7) 108.5(4) yes . . . N(4) C(6) C(9) 124.8(4) yes . . . C(7) C(6) C(9) 126.6(4) yes . . . C(6) C(7) C(8) 107.1(4) yes . . . N(3) C(8) C(7) 107.7(4) yes . . . N(3) C(8) C(10) 122.9(4) yes . . . C(7) C(8) C(10) 129.3(4) yes . . . N(6) C(11) C(12) 108.8(3) yes . . . N(6) C(11) C(14) 126.1(4) yes . . . C(12) C(11) C(14) 125.2(4) yes . . . C(11) C(12) C(13) 107.7(4) yes . . . N(5) C(13) C(12) 107.1(4) yes . . . N(5) C(13) C(15) 122.6(4) yes . . . C(12) C(13) C(15) 130.3(4) yes . . . N(7) C(16) C(17) 178.9(5) yes . . . O(1) C(18) C(19) 103.7(18) yes . . . O(2) C(19) C(22) 112.3(19) yes . . . C(18) C(19) C(20) 92.5(14) yes . . . C(19) C(20) C(21) 105.7(18) yes . . . O(1) C(21) C(20) 107(2) yes . . . C(19) C(22) C(23) 95(2) yes . . . C(22) C(23) C(24) 103(2) yes . . . O(2) C(24) C(23) 110(2) yes . . . N(1) B(1) N(3) 109.2(3) yes . . . N(1) B(1) N(5) 109.0(3) yes . . . N(3) B(1) N(5) 107.4(3) yes . . . C(1) C(2) H(2) 126.6 no . . . C(3) C(2) H(2) 126.9 no . . . C(1) C(4) H(3) 109.6 no . . . C(1) C(4) H(4) 109.7 no . . . C(1) C(4) H(5) 109.1 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 . . . C(3) C(5) H(6) 109.6 no . . . C(3) C(5) H(7) 109.6 no . . . C(3) C(5) H(8) 109.3 no . . . H(6) C(5) H(7) 109.5 no . . . H(6) C(5) H(8) 109.5 no . . . H(7) C(5) H(8) 109.5 no . . . C(6) C(7) H(9) 126.4 no . . . C(8) C(7) H(9) 126.4 no . . . C(6) C(9) H(10) 109.4 no . . . C(6) C(9) H(11) 109.3 no . . . C(6) C(9) H(12) 109.8 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(8) C(10) H(13) 109.7 no . . . C(8) C(10) H(14) 109.5 no . . . C(8) C(10) H(15) 109.2 no . . . H(13) C(10) H(14) 109.5 no . . . H(13) C(10) H(15) 109.5 no . . . H(14) C(10) H(15) 109.5 no . . . C(11) C(12) H(16) 126.2 no . . . C(13) C(12) H(16) 126.1 no . . . C(11) C(14) H(17) 109.5 no . . . C(11) C(14) H(18) 109.3 no . . . C(11) C(14) H(19) 109.6 no . . . H(17) C(14) H(18) 109.5 no . . . H(17) C(14) H(19) 109.5 no . . . H(18) C(14) H(19) 109.5 no . . . C(13) C(15) H(20) 109.6 no . . . C(13) C(15) H(21) 109.1 no . . . C(13) C(15) H(22) 109.7 no . . . H(20) C(15) H(21) 109.5 no . . . H(20) C(15) H(22) 109.5 no . . . H(21) C(15) H(22) 109.5 no . . . C(16) C(17) H(23) 109.3 no . . . C(16) C(17) H(24) 109.4 no . . . C(16) C(17) H(25) 109.7 no . . . H(23) C(17) H(24) 109.5 no . . . H(23) C(17) H(25) 109.5 no . . . H(24) C(17) H(25) 109.5 no . . . N(1) B(1) H(1) 112(3) no . . . N(3) B(1) H(1) 114(3) no . . . N(5) B(1) H(1) 105(3) no . . . #===END #============================================================================== data___[TpsRhH(SC6H4-2-COOH)]_THF _database_code_depnum_ccdc_archive 'CCDC 759754' #TrackingRef 'CIF-TpsRh1.txt' _audit_creation_date 2009-08-09 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H36 B N6 O3 Rh S ' _chemical_formula_moiety 'C26 H36 B N6 O3 Rh S ' _chemical_formula_weight 626.38 _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 10.137(2) _cell_length_b 18.086(3) _cell_length_c 15.833(3) _cell_angle_alpha 90.0000 _cell_angle_beta 102.7935(8) _cell_angle_gamma 90.0000 _cell_volume 2830.6(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9164 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 113.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296.00 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.886 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_ambient_temperature 113.1 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 22692 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.87 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _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). The minor part of the disordered methyl hydrogens bonded to C(15) were refined with restraints of bond distances (d(C-H) = 0.95) and angles (109 deg). ; _reflns_number_total 6749 _reflns_number_gt 5550 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0527 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6749 _refine_ls_number_parameters 509 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0038 _refine_diff_density_max 1.00 _refine_diff_density_min -0.63 _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) ; B B 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; 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) ; #============================================================================== # 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 Rh(1) Rh 0.282240(10) 0.331660(10) 0.223810(10) 0.01529(3) Uani 1.00 1 d . . . S(1) S 0.29536(5) 0.27833(3) 0.35693(3) 0.02191(12) Uani 1.00 1 d . . . O(1) O 0.19716(13) 0.42610(7) 0.25872(8) 0.0188(3) Uani 1.00 1 d . . . O(2) O 0.10203(15) 0.51054(7) 0.32493(10) 0.0248(3) Uani 1.00 1 d . . . O(3) O 0.12890(15) 0.59688(7) 0.19713(10) 0.0309(4) Uani 1.00 1 d . . . N(1) N 0.38441(15) 0.37750(8) 0.06894(10) 0.0176(4) Uani 1.00 1 d . . . N(2) N 0.27052(15) 0.37739(8) 0.10220(10) 0.0165(3) Uani 1.00 1 d . . . N(3) N 0.47360(16) 0.25797(8) 0.13888(10) 0.0195(4) Uani 1.00 1 d . . . N(4) N 0.37092(16) 0.24401(8) 0.18083(10) 0.0185(4) Uani 1.00 1 d . . . N(5) N 0.56526(16) 0.37850(8) 0.20677(10) 0.0181(4) Uani 1.00 1 d . . . N(6) N 0.48021(16) 0.38484(8) 0.26280(10) 0.0186(4) Uani 1.00 1 d . . . C(1) C 0.17092(19) 0.40918(9) 0.04372(12) 0.0180(4) Uani 1.00 1 d . . . C(2) C 0.2218(2) 0.43016(10) -0.02802(13) 0.0203(5) Uani 1.00 1 d . . . C(3) C 0.3559(2) 0.40946(9) -0.01023(12) 0.0187(4) Uani 1.00 1 d . . . C(4) C 0.0318(2) 0.41639(13) 0.05917(15) 0.0250(5) Uani 1.00 1 d . . . C(5) C 0.4584(2) 0.41708(13) -0.06476(14) 0.0244(5) Uani 1.00 1 d . . . C(6) C 0.3521(2) 0.17017(10) 0.18059(13) 0.0216(4) Uani 1.00 1 d . . . C(7) C 0.4453(2) 0.13727(11) 0.13928(15) 0.0272(5) Uani 1.00 1 d . . . C(8) C 0.5194(2) 0.19295(11) 0.11360(14) 0.0246(5) Uani 1.00 1 d . . . C(9) C 0.2443(2) 0.13395(13) 0.21657(17) 0.0281(6) Uani 1.00 1 d . . . C(10) C 0.6314(2) 0.18873(14) 0.06628(18) 0.0335(6) Uani 1.00 1 d . . . C(11) C 0.5471(2) 0.42269(10) 0.33154(13) 0.0202(4) Uani 1.00 1 d . . . C(12) C 0.6761(2) 0.43989(11) 0.32037(14) 0.0230(5) Uani 1.00 1 d . . . C(13) C 0.6855(2) 0.41135(10) 0.24125(13) 0.0210(4) Uani 1.00 1 d . . . C(14) C 0.4841(2) 0.44311(12) 0.40509(14) 0.0247(5) Uani 1.00 1 d . . . C(15) C 0.8004(2) 0.41244(14) 0.19694(16) 0.0283(6) Uani 1.00 1 d . . . C(16) C 0.17834(19) 0.32132(10) 0.40634(12) 0.0184(4) Uani 1.00 1 d . . . C(17) C 0.11687(19) 0.39201(10) 0.38749(12) 0.0180(4) Uani 1.00 1 d . . . C(18) C 0.0262(2) 0.41770(11) 0.43683(13) 0.0232(5) Uani 1.00 1 d . . . C(19) C -0.0060(2) 0.37597(12) 0.50209(14) 0.0290(5) Uani 1.00 1 d . . . C(20) C 0.0556(2) 0.30720(12) 0.52117(14) 0.0278(5) Uani 1.00 1 d . . . C(21) C 0.1453(2) 0.28157(11) 0.47544(13) 0.0241(5) Uani 1.00 1 d . . . C(22) C 0.14339(19) 0.44137(10) 0.31919(12) 0.0179(4) Uani 1.00 1 d . . . C(23) C 0.0735(2) 0.67058(13) 0.20074(18) 0.0340(6) Uani 1.00 1 d . . . C(24) C 0.1806(2) 0.72390(13) 0.18646(17) 0.0333(6) Uani 1.00 1 d . . . C(25) C 0.2584(3) 0.67910(14) 0.1330(2) 0.0456(8) Uani 1.00 1 d . . . C(26) C 0.2550(2) 0.60166(13) 0.16929(17) 0.0326(6) Uani 1.00 1 d . . . B(1) B 0.5136(2) 0.33814(12) 0.12038(15) 0.0196(5) Uani 1.00 1 d . . . H(1) H 0.5879(18) 0.3364(9) 0.0821(12) 0.015(4) Uiso 1.00 1 d . . . H(2) H 0.174(2) 0.4537(11) -0.0779(14) 0.031(6) Uiso 1.00 1 d . . . H(3) H 0.029(2) 0.4551(12) 0.0977(15) 0.037(6) Uiso 1.00 1 d . . . H(4) H -0.035(2) 0.4256(12) 0.0045(15) 0.035(6) Uiso 1.00 1 d . . . H(5) H 0.005(2) 0.3739(13) 0.0846(16) 0.043(7) Uiso 1.00 1 d . . . H(6) H 0.541(2) 0.4323(11) -0.0318(14) 0.029(6) Uiso 1.00 1 d . . . H(7) H 0.432(2) 0.4531(12) -0.1077(15) 0.037(6) Uiso 1.00 1 d . . . H(8) H 0.467(2) 0.3700(13) -0.0943(16) 0.044(7) Uiso 1.00 1 d . . . H(9) H 0.456(2) 0.0856(11) 0.1310(13) 0.023(5) Uiso 1.00 1 d . . . H(10) H 0.190(4) 0.097(2) 0.170(2) 0.020(9) Uiso 0.55 1 d P . . H(11) H 0.283(5) 0.105(3) 0.263(3) 0.047(17) Uiso 0.55 1 d P . . H(12) H 0.187(4) 0.168(2) 0.235(2) 0.014(9) Uiso 0.55 1 d P . . H(13) H 0.603(2) 0.2066(13) 0.0113(17) 0.045(7) Uiso 1.00 1 d . . . H(14) H 0.664(2) 0.1413(13) 0.0656(15) 0.040(6) Uiso 1.00 1 d . . . H(15) H 0.712(2) 0.2191(11) 0.0921(14) 0.031(6) Uiso 1.00 1 d . . . H(16) H 0.740(2) 0.4635(11) 0.3582(14) 0.029(6) Uiso 1.00 1 d . . . H(17) H 0.553(2) 0.4609(10) 0.4506(13) 0.024(5) Uiso 1.00 1 d . . . H(18) H 0.445(2) 0.4016(12) 0.4269(15) 0.039(6) Uiso 1.00 1 d . . . H(19) H 0.416(2) 0.4807(11) 0.3908(13) 0.025(5) Uiso 1.00 1 d . . . H(20) H 0.858(3) 0.4526(18) 0.216(2) 0.042(10) Uiso 0.80 1 d P . . H(21) H 0.769(2) 0.4199(16) 0.1299(18) 0.022(8) Uiso 0.80 1 d P . . H(22) H 0.853(3) 0.3723(19) 0.207(2) 0.044(10) Uiso 0.80 1 d P . . H(23) H -0.012(2) 0.4646(11) 0.4236(13) 0.025(5) Uiso 1.00 1 d . . . H(24) H -0.073(2) 0.3949(11) 0.5323(14) 0.031(6) Uiso 1.00 1 d . . . H(25) H 0.033(2) 0.2774(11) 0.5635(14) 0.029(6) Uiso 1.00 1 d . . . H(26) H 0.190(2) 0.2362(11) 0.4879(14) 0.028(5) Uiso 1.00 1 d . . . H(27) H 0.114(2) 0.5352(13) 0.2864(16) 0.041(7) Uiso 1.00 1 d . . . H(28) H 0.1401(17) 0.2918(9) 0.1963(11) 0.011(4) Uiso 1.00 1 d . . . H(29) H 0.054(2) 0.6754(12) 0.2570(16) 0.041(7) Uiso 1.00 1 d . . . H(30) H -0.007(2) 0.6726(13) 0.1592(17) 0.053(8) Uiso 1.00 1 d . . . H(31) H 0.238(2) 0.7371(13) 0.2413(17) 0.048(7) Uiso 1.00 1 d . . . H(32) H 0.148(2) 0.7671(13) 0.1573(15) 0.039(6) Uiso 1.00 1 d . . . H(33) H 0.350(2) 0.6957(13) 0.1386(16) 0.047(7) Uiso 1.00 1 d . . . H(34) H 0.209(3) 0.6821(17) 0.070(2) 0.093(12) Uiso 1.00 1 d . . . H(35) H 0.328(2) 0.5912(12) 0.2207(15) 0.039(6) Uiso 1.00 1 d . . . H(36) H 0.253(2) 0.5627(12) 0.1278(15) 0.039(6) Uiso 1.00 1 d . . . H(37) H 0.238(4) 0.156(2) 0.276(3) 0.012(11) Uiso 0.45 1 d P . . H(38) H 0.154(5) 0.141(3) 0.179(3) 0.028(13) Uiso 0.45 1 d P . . H(39) H 0.266(7) 0.082(3) 0.233(5) 0.05(2) Uiso 0.45 1 d P . . H(40) H 0.814(7) 0.3642(16) 0.177(6) 0.04(3) Uiso 0.20 1 d P . . H(41) H 0.879(3) 0.429(6) 0.236(2) 0.04(3) Uiso 0.20 1 d P . . H(42) H 0.780(5) 0.445(5) 0.149(4) 0.04(3) Uiso 0.20 1 d P . . 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) 0.01676(8) 0.01251(7) 0.01761(8) 0.00147(6) 0.00597(6) -0.00043(6) S(1) 0.0272(2) 0.0168(2) 0.0233(2) 0.0048(2) 0.0089(2) 0.00438(19) O(1) 0.0228(7) 0.0157(6) 0.0204(7) 0.0033(5) 0.0103(5) 0.0008(5) O(2) 0.0372(8) 0.0153(6) 0.0262(8) 0.0069(6) 0.0163(6) 0.0029(6) O(3) 0.0330(8) 0.0252(7) 0.0388(9) 0.0080(6) 0.0174(7) 0.0103(6) N(1) 0.0178(8) 0.0172(7) 0.0193(8) 0.0004(6) 0.0071(6) -0.0022(6) N(2) 0.0160(7) 0.0158(7) 0.0195(8) 0.0008(6) 0.0076(6) -0.0031(6) N(3) 0.0184(8) 0.0193(7) 0.0216(8) 0.0031(6) 0.0060(6) -0.0037(6) N(4) 0.0177(8) 0.0174(7) 0.0205(8) 0.0013(6) 0.0044(6) -0.0023(6) N(5) 0.0162(8) 0.0174(7) 0.0215(8) -0.0001(6) 0.0060(6) -0.0008(6) N(6) 0.0201(8) 0.0172(7) 0.0193(8) -0.0002(6) 0.0064(6) -0.0026(6) C(1) 0.0204(9) 0.0124(8) 0.0219(10) 0.0029(7) 0.0058(8) -0.0014(7) C(2) 0.0226(10) 0.0177(9) 0.0207(10) 0.0023(7) 0.0050(8) 0.0020(7) C(3) 0.0239(10) 0.0134(8) 0.0197(9) -0.0020(7) 0.0068(8) -0.0025(7) C(4) 0.0229(11) 0.0252(11) 0.0281(12) 0.0057(9) 0.0082(9) 0.0057(9) C(5) 0.0246(11) 0.0279(11) 0.0229(11) -0.0032(9) 0.0103(9) -0.0017(9) C(6) 0.0220(10) 0.0164(8) 0.0236(10) 0.0010(8) -0.0008(8) -0.0026(8) C(7) 0.0274(11) 0.0178(10) 0.0347(12) 0.0065(8) 0.0035(9) -0.0063(8) C(8) 0.0213(10) 0.0232(9) 0.0278(11) 0.0057(8) 0.0025(8) -0.0090(8) C(9) 0.0331(13) 0.0172(11) 0.0342(13) 0.0001(9) 0.0077(11) -0.0004(9) C(10) 0.0287(12) 0.0306(12) 0.0437(15) 0.0070(10) 0.0134(11) -0.0127(11) C(11) 0.0265(10) 0.0130(8) 0.0201(9) -0.0000(7) 0.0030(8) 0.0008(7) C(12) 0.0226(10) 0.0203(9) 0.0240(10) -0.0038(8) 0.0004(8) -0.0002(8) C(13) 0.0199(10) 0.0160(9) 0.0259(10) -0.0004(7) 0.0026(8) 0.0035(8) C(14) 0.0322(12) 0.0201(10) 0.0219(10) -0.0045(9) 0.0060(9) -0.0034(8) C(15) 0.0201(11) 0.0299(12) 0.0351(13) -0.0025(9) 0.0066(9) 0.0060(10) C(16) 0.0212(9) 0.0164(9) 0.0170(9) -0.0021(7) 0.0029(7) -0.0012(7) C(17) 0.0210(10) 0.0173(8) 0.0155(9) -0.0011(7) 0.0039(7) -0.0002(7) C(18) 0.0268(11) 0.0231(10) 0.0204(10) 0.0024(8) 0.0069(8) -0.0001(8) C(19) 0.0343(12) 0.0337(12) 0.0224(10) -0.0019(10) 0.0133(9) -0.0034(9) C(20) 0.0362(12) 0.0295(11) 0.0189(10) -0.0085(9) 0.0087(9) 0.0023(8) C(21) 0.0317(11) 0.0200(10) 0.0193(10) -0.0021(8) 0.0031(8) 0.0021(8) C(22) 0.0181(9) 0.0158(8) 0.0195(9) 0.0019(7) 0.0034(7) -0.0001(7) C(23) 0.0312(13) 0.0279(11) 0.0452(14) 0.0094(10) 0.0134(11) 0.0086(11) C(24) 0.0355(13) 0.0259(11) 0.0378(14) 0.0008(10) 0.0065(11) -0.0001(10) C(25) 0.0498(17) 0.0366(14) 0.0601(19) -0.0068(12) 0.0332(15) 0.0003(13) C(26) 0.0302(13) 0.0308(12) 0.0402(14) 0.0017(9) 0.0149(11) -0.0035(10) B(1) 0.0161(10) 0.0213(10) 0.0220(11) 0.0019(8) 0.0058(8) -0.0036(9) #============================================================================== _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 Rh(1) S(1) 2.2948(5) yes . . Rh(1) O(1) 2.0440(13) yes . . Rh(1) N(2) 2.0746(15) yes . . Rh(1) N(4) 2.0137(15) yes . . Rh(1) N(6) 2.1874(15) yes . . S(1) C(16) 1.742(2) yes . . O(1) C(22) 1.233(2) yes . . O(2) C(22) 1.329(2) yes . . O(3) C(23) 1.453(2) yes . . O(3) C(26) 1.444(3) yes . . N(1) N(2) 1.371(2) yes . . N(1) C(3) 1.352(2) yes . . N(1) B(1) 1.553(2) yes . . N(2) C(1) 1.339(2) yes . . N(3) N(4) 1.376(2) yes . . N(3) C(8) 1.357(2) yes . . N(3) B(1) 1.551(2) yes . . N(4) C(6) 1.349(2) yes . . N(5) N(6) 1.372(2) yes . . N(5) C(13) 1.357(2) yes . . N(5) B(1) 1.536(2) yes . . N(6) C(11) 1.336(2) yes . . C(1) C(2) 1.400(3) yes . . C(1) C(4) 1.490(3) yes . . C(2) C(3) 1.377(2) yes . . C(3) C(5) 1.497(3) yes . . C(6) C(7) 1.395(3) yes . . C(6) C(9) 1.491(3) yes . . C(7) C(8) 1.371(3) yes . . C(8) C(10) 1.494(3) yes . . C(11) C(12) 1.393(3) yes . . C(11) C(14) 1.493(3) yes . . C(12) C(13) 1.377(3) yes . . C(13) C(15) 1.486(3) yes . . C(16) C(17) 1.425(2) yes . . C(16) C(21) 1.410(2) yes . . C(17) C(18) 1.411(3) yes . . C(17) C(22) 1.472(2) yes . . C(18) C(19) 1.376(3) yes . . C(19) C(20) 1.395(3) yes . . C(20) C(21) 1.363(3) yes . . C(23) C(24) 1.506(3) yes . . C(24) C(25) 1.513(4) yes . . C(25) C(26) 1.517(3) yes . . Rh(1) H(28) 1.583(16) no . . O(2) H(27) 0.79(2) no . . C(2) H(2) 0.93(2) no . . C(4) H(3) 0.93(2) no . . C(4) H(4) 0.99(2) no . . C(4) H(5) 0.93(2) no . . C(5) H(6) 0.92(2) no . . C(5) H(7) 0.94(2) no . . C(5) H(8) 0.98(2) no . . C(7) H(9) 0.95(2) no . . C(9) H(10) 1.05(3) no . . C(9) H(11) 0.91(6) no . . C(9) H(12) 0.93(4) no . . C(9) H(37) 1.04(5) no . . C(9) H(38) 0.98(4) no . . C(9) H(39) 0.99(7) no . . C(10) H(13) 0.91(2) no . . C(10) H(14) 0.92(2) no . . C(10) H(15) 0.99(2) no . . C(12) H(16) 0.89(2) no . . C(14) H(17) 0.944(19) no . . C(14) H(18) 0.95(2) no . . C(14) H(19) 0.96(2) no . . C(15) H(20) 0.94(3) no . . C(15) H(21) 1.05(2) no . . C(15) H(22) 0.89(3) no . . C(15) H(40) 0.95(4) no . . C(15) H(41) 0.95(5) no . . C(15) H(42) 0.95(8) no . . C(18) H(23) 0.94(2) no . . C(19) H(24) 0.97(2) no . . C(20) H(25) 0.93(2) no . . C(21) H(26) 0.94(2) no . . C(23) H(29) 0.96(2) no . . C(23) H(30) 0.93(2) no . . C(24) H(31) 0.96(2) no . . C(24) H(32) 0.93(2) no . . C(25) H(33) 0.96(2) no . . C(25) H(34) 1.01(3) no . . C(26) H(35) 0.99(2) no . . C(26) H(36) 0.96(2) no . . B(1) H(1) 1.07(2) 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 S(1) Rh(1) O(1) 92.58(3) yes . . . S(1) Rh(1) N(2) 178.64(4) yes . . . S(1) Rh(1) N(4) 92.30(4) yes . . . S(1) Rh(1) N(6) 93.59(4) yes . . . O(1) Rh(1) N(2) 88.68(5) yes . . . O(1) Rh(1) N(4) 174.80(6) yes . . . O(1) Rh(1) N(6) 88.39(5) yes . . . N(2) Rh(1) N(4) 86.47(6) yes . . . N(2) Rh(1) N(6) 86.96(5) yes . . . N(4) Rh(1) N(6) 89.50(6) yes . . . Rh(1) S(1) C(16) 108.55(6) yes . . . Rh(1) O(1) C(22) 133.04(12) yes . . . C(23) O(3) C(26) 109.46(16) yes . . . N(2) N(1) C(3) 109.35(14) yes . . . N(2) N(1) B(1) 118.81(15) yes . . . C(3) N(1) B(1) 131.64(17) yes . . . Rh(1) N(2) N(1) 118.49(10) yes . . . Rh(1) N(2) C(1) 133.82(14) yes . . . N(1) N(2) C(1) 107.69(15) yes . . . N(4) N(3) C(8) 109.16(15) yes . . . N(4) N(3) B(1) 121.33(15) yes . . . C(8) N(3) B(1) 129.32(18) yes . . . Rh(1) N(4) N(3) 117.42(10) yes . . . Rh(1) N(4) C(6) 135.00(14) yes . . . N(3) N(4) C(6) 107.56(15) yes . . . N(6) N(5) C(13) 109.90(15) yes . . . N(6) N(5) B(1) 118.44(15) yes . . . C(13) N(5) B(1) 131.66(18) yes . . . Rh(1) N(6) N(5) 116.70(10) yes . . . Rh(1) N(6) C(11) 136.33(14) yes . . . N(5) N(6) C(11) 106.94(15) yes . . . N(2) C(1) C(2) 108.69(17) yes . . . N(2) C(1) C(4) 121.36(18) yes . . . C(2) C(1) C(4) 129.94(16) yes . . . C(1) C(2) C(3) 106.53(16) yes . . . N(1) C(3) C(2) 107.73(18) yes . . . N(1) C(3) C(5) 122.72(16) yes . . . C(2) C(3) C(5) 129.53(17) yes . . . N(4) C(6) C(7) 108.28(18) yes . . . N(4) C(6) C(9) 123.28(19) yes . . . C(7) C(6) C(9) 128.39(18) yes . . . C(6) C(7) C(8) 107.34(18) yes . . . N(3) C(8) C(7) 107.64(19) yes . . . N(3) C(8) C(10) 122.68(19) yes . . . C(7) C(8) C(10) 129.7(2) yes . . . N(6) C(11) C(12) 109.40(19) yes . . . N(6) C(11) C(14) 122.29(18) yes . . . C(12) C(11) C(14) 128.28(17) yes . . . C(11) C(12) C(13) 106.71(17) yes . . . N(5) C(13) C(12) 107.05(18) yes . . . N(5) C(13) C(15) 122.92(18) yes . . . C(12) C(13) C(15) 130.03(18) yes . . . S(1) C(16) C(17) 128.04(15) yes . . . S(1) C(16) C(21) 115.04(14) yes . . . C(17) C(16) C(21) 116.88(18) yes . . . C(16) C(17) C(18) 119.22(18) yes . . . C(16) C(17) C(22) 123.75(18) yes . . . C(18) C(17) C(22) 117.03(16) yes . . . C(17) C(18) C(19) 121.82(18) yes . . . C(18) C(19) C(20) 118.8(2) yes . . . C(19) C(20) C(21) 120.5(2) yes . . . C(16) C(21) C(20) 122.67(18) yes . . . O(1) C(22) O(2) 117.66(17) yes . . . O(1) C(22) C(17) 128.20(16) yes . . . O(2) C(22) C(17) 114.14(17) yes . . . O(3) C(23) C(24) 106.5(2) yes . . . C(23) C(24) C(25) 102.9(2) yes . . . C(24) C(25) C(26) 103.0(2) yes . . . O(3) C(26) C(25) 105.5(2) yes . . . N(1) B(1) N(3) 107.59(14) yes . . . N(1) B(1) N(5) 109.31(16) yes . . . N(3) B(1) N(5) 109.14(16) yes . . . S(1) Rh(1) H(28) 85.7(6) no . . . O(1) Rh(1) H(28) 92.4(6) no . . . N(2) Rh(1) H(28) 93.7(6) no . . . N(4) Rh(1) H(28) 89.8(6) no . . . N(6) Rh(1) H(28) 179.0(6) no . . . C(22) O(2) H(27) 112.2(18) no . . . C(1) C(2) H(2) 126.3(15) no . . . C(3) C(2) H(2) 127.2(15) no . . . C(1) C(4) H(3) 109.9(14) no . . . C(1) C(4) H(4) 111.2(15) no . . . C(1) C(4) H(5) 111.9(15) no . . . H(3) C(4) H(4) 109.4(18) no . . . H(3) C(4) H(5) 106(2) no . . . H(4) C(4) H(5) 108.0(19) no . . . C(3) C(5) H(6) 110.9(15) no . . . C(3) C(5) H(7) 111.2(15) no . . . C(3) C(5) H(8) 110.0(15) no . . . H(6) C(5) H(7) 106.2(19) no . . . H(6) C(5) H(8) 111.1(19) no . . . H(7) C(5) H(8) 107(2) no . . . C(6) C(7) H(9) 126.1(13) no . . . C(8) C(7) H(9) 126.6(13) no . . . C(6) C(9) H(10) 109(2) no . . . C(6) C(9) H(11) 110(3) no . . . C(6) C(9) H(12) 113(2) no . . . C(6) C(9) H(37) 112(2) no . . . C(6) C(9) H(38) 112(3) no . . . C(6) C(9) H(39) 112(4) no . . . H(10) C(9) H(11) 105(4) no . . . H(10) C(9) H(12) 111(3) no . . . H(11) C(9) H(12) 109(4) no . . . H(37) C(9) H(38) 105(4) no . . . H(37) C(9) H(39) 100(5) no . . . H(38) C(9) H(39) 114(5) no . . . C(8) C(10) H(13) 110.4(17) no . . . C(8) C(10) H(14) 111.4(16) no . . . C(8) C(10) H(15) 114.2(14) no . . . H(13) C(10) H(14) 111(2) no . . . H(13) C(10) H(15) 105(2) no . . . H(14) C(10) H(15) 105.1(18) no . . . C(11) C(12) H(16) 125.7(16) no . . . C(13) C(12) H(16) 127.6(16) no . . . C(11) C(14) H(17) 107.7(14) no . . . C(11) C(14) H(18) 112.0(15) no . . . C(11) C(14) H(19) 113.6(13) no . . . H(17) C(14) H(18) 107.1(18) no . . . H(17) C(14) H(19) 108.3(17) no . . . H(18) C(14) H(19) 107.9(19) no . . . C(13) C(15) H(20) 110(2) no . . . C(13) C(15) H(21) 112.6(15) no . . . C(13) C(15) H(22) 114(2) no . . . C(13) C(15) H(40) 109(5) no . . . C(13) C(15) H(41) 109(2) no . . . C(13) C(15) H(42) 109(3) no . . . H(20) C(15) H(21) 105(2) no . . . H(20) C(15) H(22) 106(2) no . . . H(21) C(15) H(22) 109(2) no . . . H(40) C(15) H(41) 109(7) no . . . H(40) C(15) H(42) 109(8) no . . . H(41) C(15) H(42) 109(6) no . . . C(17) C(18) H(23) 117.7(14) no . . . C(19) C(18) H(23) 120.5(14) no . . . C(18) C(19) H(24) 118.8(12) no . . . C(20) C(19) H(24) 122.3(12) no . . . C(19) C(20) H(25) 120.4(14) no . . . C(21) C(20) H(25) 119.0(14) no . . . C(16) C(21) H(26) 115.2(14) no . . . C(20) C(21) H(26) 122.1(14) no . . . O(3) C(23) H(29) 106.3(13) no . . . O(3) C(23) H(30) 107.1(15) no . . . C(24) C(23) H(29) 112.6(13) no . . . C(24) C(23) H(30) 114.6(17) no . . . H(29) C(23) H(30) 109(2) no . . . C(23) C(24) H(31) 109.7(16) no . . . C(23) C(24) H(32) 115.2(15) no . . . C(25) C(24) H(31) 110.5(16) no . . . C(25) C(24) H(32) 110.0(16) no . . . H(31) C(24) H(32) 108(2) no . . . C(24) C(25) H(33) 113.1(15) no . . . C(24) C(25) H(34) 109(2) no . . . C(26) C(25) H(33) 110.9(14) no . . . C(26) C(25) H(34) 112.0(18) no . . . H(33) C(25) H(34) 109(2) no . . . O(3) C(26) H(35) 106.8(15) no . . . O(3) C(26) H(36) 106.2(15) no . . . C(25) C(26) H(35) 114.4(13) no . . . C(25) C(26) H(36) 114.7(15) no . . . H(35) C(26) H(36) 108.7(19) no . . . N(1) B(1) H(1) 109.6(9) no . . . N(3) B(1) H(1) 109.0(9) no . . . N(5) B(1) H(1) 112.1(9) no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) O(3) 3.2667(17) ? . . O(2) O(3) 2.617(2) ? . . O(3) H(27) 1.83(2) ? . . #===END