Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _audit_creation_date 'Mon Mar 13 17:46:22 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ _journal_coden_Cambridge 186 loop_ _publ_author_name 'Tobita, Hiromi' 'Ogino, H.' 'Ohshitanai, Shin' 'Okazaki, Masaaki' # SUBMISSION DETAILS _publ_contact_author_name 'Prof Hiromi Tobita' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science Tohoku University Aramaki-aza-Aoba, Aoba-ku Sendai Miyagi 980-8578 JAPAN ; _publ_contact_author_email 'TOBITA@INORG.CHEM.TOHOKU.AC.JP' _publ_contact_author_fax '81-22-217-6543' _publ_contact_author_phone '81-22-217-6541' _publ_requested_journal 'Dalton' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ _publ_section_title ; Synthesis and Structure of {(2-Phosphinoethyl)silyl}rhodium(I) Complex Rh[(k2-Si,P)-Me2Si(CH2)2PPh2](PMe3)n (n = 2, 3) ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ data_complex_1 _database_code_CSD 173810 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C22 H39 Cl P3 Rh Si ' _chemical_formula_moiety 'C22 H39 Cl P3 Rh Si ' _chemical_formula_weight 562.92 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbca' _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 15.1621(8) _cell_length_b 25.695(1) _cell_length_c 13.5872(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5293.5(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 56059 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.898 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22911 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9911 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9911 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # 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 6018 _reflns_number_gt 5110 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.2145 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6018 _refine_ls_number_parameters 257 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.16300(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0686 _refine_diff_density_max 1.47 _refine_diff_density_min -1.28 _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) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.082 0.070 ;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) ; '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 Rh 0.25361(2) 0.09731(1) 0.10842(2) 0.0165(1) Uani 1.00 d . . . Cl Cl 0.39371(6) 0.06108(4) 0.18377(8) 0.0278(2) Uani 1.00 d . . . P1 P 0.33298(6) 0.16158(4) 0.03192(7) 0.0184(2) Uani 1.00 d . . . P2 P 0.18786(7) 0.01786(4) 0.13724(8) 0.0238(3) Uani 1.00 d . . . P3 P 0.21141(7) 0.13749(4) 0.25790(7) 0.0212(2) Uani 1.00 d . . . Si Si 0.13525(7) 0.12807(4) 0.01564(8) 0.0208(3) Uani 1.00 d . . . C1 C 0.1730(3) 0.1919(2) -0.0413(3) 0.0264(10) Uani 1.00 d . . . C2 C 0.2703(3) 0.1864(2) -0.0725(3) 0.0241(9) Uani 1.00 d . . . C3 C 0.0261(3) 0.1434(2) 0.0759(4) 0.033(1) Uani 1.00 d . . . C4 C 0.1064(3) 0.0870(2) -0.0946(3) 0.033(1) Uani 1.00 d . . . C5 C 0.3640(3) 0.2199(1) 0.1001(3) 0.0202(9) Uani 1.00 d . . . C6 C 0.3344(3) 0.2699(2) 0.0768(3) 0.0276(10) Uani 1.00 d . . . C7 C 0.3598(3) 0.3124(1) 0.1339(3) 0.031(1) Uani 1.00 d . . . C8 C 0.4152(3) 0.3062(2) 0.2120(3) 0.031(1) Uani 1.00 d . . . C9 C 0.4446(3) 0.2568(2) 0.2368(3) 0.030(1) Uani 1.00 d . . . C10 C 0.4192(3) 0.2140(1) 0.1807(3) 0.0238(9) Uani 1.00 d . . . C11 C 0.4390(3) 0.1432(2) -0.0235(3) 0.0224(9) Uani 1.00 d . . . C12 C 0.5034(3) 0.1807(2) -0.0418(3) 0.0245(9) Uani 1.00 d . . . C13 C 0.5811(3) 0.1673(2) -0.0922(3) 0.030(1) Uani 1.00 d . . . C14 C 0.5936(3) 0.1171(2) -0.1244(3) 0.034(1) Uani 1.00 d . . . C15 C 0.5306(3) 0.0788(2) -0.1045(3) 0.035(1) Uani 1.00 d . . . C16 C 0.4538(3) 0.0923(2) -0.0546(3) 0.030(1) Uani 1.00 d . . . C17 C 0.2220(4) -0.0160(2) 0.2480(4) 0.036(1) Uani 1.00 d . . . C18 C 0.2188(4) -0.0292(2) 0.0426(4) 0.040(1) Uani 1.00 d . . . C19 C 0.0690(3) 0.0089(2) 0.1416(4) 0.035(1) Uani 1.00 d . . . C20 C 0.2920(3) 0.1355(2) 0.3573(3) 0.030(1) Uani 1.00 d . . . C21 C 0.1849(3) 0.2064(2) 0.2562(3) 0.032(1) Uani 1.00 d . . . C22 C 0.1153(3) 0.1115(2) 0.3218(3) 0.033(1) Uani 1.00 d . . . H1 H 0.258(4) 0.077(4) -0.012(6) 0.069(9) Uiso 1.00 calc . . . H2 H 0.1378 0.1994 -0.0983 0.0304 Uiso 1.00 calc . . . H3 H 0.1671 0.2193 0.0044 0.0304 Uiso 1.00 calc . . . H4 H 0.2921 0.2192 -0.0919 0.0274 Uiso 1.00 calc . . . H5 H 0.2740 0.1626 -0.1261 0.0274 Uiso 1.00 calc . . . H6 H 0.0348 0.1700 0.1240 0.0371 Uiso 1.00 calc . . . H7 H -0.0140 0.1558 0.0273 0.0371 Uiso 1.00 calc . . . H8 H 0.0035 0.1133 0.1061 0.0371 Uiso 1.00 calc . . . H9 H 0.0623 0.1033 -0.1326 0.0379 Uiso 1.00 calc . . . H10 H 0.1583 0.0825 -0.1350 0.0379 Uiso 1.00 calc . . . H11 H 0.0870 0.0536 -0.0740 0.0379 Uiso 1.00 calc . . . H12 H 0.2959 0.2750 0.0217 0.0325 Uiso 1.00 calc . . . H13 H 0.3385 0.3463 0.1181 0.0381 Uiso 1.00 calc . . . H14 H 0.4327 0.3353 0.2503 0.0368 Uiso 1.00 calc . . . H15 H 0.4831 0.2520 0.2926 0.0356 Uiso 1.00 calc . . . H16 H 0.4410 0.1799 0.1979 0.0278 Uiso 1.00 calc . . . H17 H 0.4948 0.2156 -0.0196 0.0279 Uiso 1.00 calc . . . H18 H 0.6246 0.1934 -0.1035 0.0353 Uiso 1.00 calc . . . H19 H 0.6448 0.1085 -0.1609 0.0390 Uiso 1.00 calc . . . H20 H 0.5409 0.0438 -0.1246 0.0413 Uiso 1.00 calc . . . H21 H 0.4111 0.0661 -0.0396 0.0351 Uiso 1.00 calc . . . H22 H 0.1942 0.0008 0.3045 0.0451 Uiso 1.00 calc . . . H23 H 0.2039 -0.0508 0.2462 0.0451 Uiso 1.00 calc . . . H24 H 0.2837 -0.0134 0.2560 0.0451 Uiso 1.00 calc . . . H25 H 0.2018 -0.0632 0.0632 0.0468 Uiso 1.00 calc . . . H26 H 0.1907 -0.0208 -0.0172 0.0468 Uiso 1.00 calc . . . H27 H 0.2813 -0.0284 0.0340 0.0468 Uiso 1.00 calc . . . H28 H 0.0465 0.0238 0.2000 0.0419 Uiso 1.00 calc . . . H29 H 0.0429 0.0246 0.0859 0.0419 Uiso 1.00 calc . . . H30 H 0.0564 -0.0277 0.1412 0.0419 Uiso 1.00 calc . . . H31 H 0.2992 0.1003 0.3788 0.0357 Uiso 1.00 calc . . . H32 H 0.3474 0.1478 0.3336 0.0357 Uiso 1.00 calc . . . H33 H 0.2729 0.1562 0.4102 0.0357 Uiso 1.00 calc . . . H34 H 0.2306 0.2257 0.2247 0.0387 Uiso 1.00 calc . . . H35 H 0.1310 0.2122 0.2207 0.0387 Uiso 1.00 calc . . . H36 H 0.1775 0.2193 0.3215 0.0387 Uiso 1.00 calc . . . H37 H 0.1001 0.1334 0.3756 0.0380 Uiso 1.00 calc . . . H38 H 0.0659 0.1105 0.2770 0.0380 Uiso 1.00 calc . . . H39 H 0.1265 0.0774 0.3445 0.0380 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 0.0123(2) 0.0174(2) 0.0200(3) 0.00007(8) -0.00080(9) -0.00066(9) Cl 0.0176(5) 0.0287(5) 0.0370(5) 0.0034(3) -0.0050(4) 0.0027(4) P1 0.0143(5) 0.0185(4) 0.0223(5) 0.0003(3) 0.0003(3) 0.0009(3) P2 0.0224(5) 0.0205(5) 0.0286(5) -0.0035(3) -0.0019(4) 0.0006(4) P3 0.0175(5) 0.0244(5) 0.0216(5) -0.0008(3) 0.0005(3) -0.0028(4) Si 0.0132(5) 0.0248(5) 0.0242(5) 0.0008(4) -0.0032(4) 0.0006(4) C1 0.019(2) 0.026(2) 0.034(2) 0.003(1) -0.004(2) 0.005(2) C2 0.021(2) 0.027(2) 0.024(2) -0.001(1) -0.002(2) 0.001(2) C3 0.022(2) 0.039(2) 0.039(2) 0.006(2) -0.002(2) 0.002(2) C4 0.032(3) 0.036(2) 0.031(2) -0.003(2) -0.011(2) -0.005(2) C5 0.015(2) 0.019(2) 0.026(2) 0.001(1) 0.005(1) 0.003(1) C6 0.031(2) 0.021(2) 0.030(2) 0.001(1) 0.001(2) 0.003(2) C7 0.038(3) 0.018(2) 0.037(2) -0.001(2) 0.003(2) -0.001(2) C8 0.033(2) 0.026(2) 0.035(2) -0.008(2) 0.006(2) -0.008(2) C9 0.028(2) 0.031(2) 0.031(2) 0.001(2) 0.000(2) -0.005(2) C10 0.019(2) 0.025(2) 0.027(2) 0.003(1) 0.000(1) 0.001(1) C11 0.017(2) 0.029(2) 0.022(2) 0.002(1) -0.001(1) 0.000(1) C12 0.019(2) 0.031(2) 0.023(2) 0.001(1) -0.001(1) 0.001(1) C13 0.019(2) 0.039(2) 0.033(2) -0.001(2) 0.004(2) 0.007(2) C14 0.022(2) 0.046(2) 0.034(2) 0.010(2) 0.008(2) 0.001(2) C15 0.026(2) 0.035(2) 0.044(3) 0.005(2) 0.008(2) -0.008(2) C16 0.027(2) 0.026(2) 0.036(2) 0.000(2) 0.004(2) -0.004(2) C17 0.038(3) 0.031(2) 0.040(2) -0.006(2) -0.008(2) 0.014(2) C18 0.051(3) 0.026(2) 0.042(3) -0.004(2) 0.005(2) -0.004(2) C19 0.024(2) 0.037(2) 0.043(3) -0.012(2) -0.005(2) 0.000(2) C20 0.027(2) 0.041(2) 0.021(2) -0.003(2) -0.004(2) -0.002(2) C21 0.032(2) 0.030(2) 0.034(2) 0.003(2) 0.001(2) -0.010(2) C22 0.028(2) 0.037(2) 0.034(2) -0.005(2) 0.010(2) -0.006(2) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF94 (PATTY)' _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 CL 2.535(1) . . yes RH P1 2.2925(9) . . yes RH P2 2.306(1) . . yes RH P3 2.366(1) . . yes RH SI 2.331(1) . . yes P1 C2 1.823(4) . . yes P1 C5 1.822(4) . . yes P1 C11 1.837(4) . . yes P2 C17 1.814(5) . . yes P2 C18 1.827(5) . . yes P2 C19 1.818(5) . . yes P3 C20 1.822(4) . . yes P3 C21 1.815(4) . . yes P3 C22 1.822(4) . . yes SI C1 1.902(4) . . yes SI C3 1.888(5) . . yes SI C4 1.883(4) . . yes C1 C2 1.542(6) . . yes C5 C6 1.398(5) . . yes C5 C10 1.386(5) . . yes C6 C7 1.394(6) . . yes C7 C8 1.364(7) . . yes C8 C9 1.386(6) . . yes C9 C10 1.392(5) . . yes C11 C12 1.393(6) . . yes C11 C16 1.393(5) . . yes C12 C13 1.405(6) . . yes C13 C14 1.375(6) . . yes C14 C15 1.398(7) . . yes C15 C16 1.392(6) . . 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 CL RH P1 90.45(3) . 1_555 1_555 yes CL RH P2 88.20(4) . 1_555 1_555 yes CL RH P3 92.31(4) . 1_555 1_555 yes CL RH SI 171.08(4) . 1_555 1_555 yes P1 RH P2 160.37(4) . 1_555 1_555 yes P1 RH P3 102.52(3) . 1_555 1_555 yes P1 RH SI 85.10(4) . 1_555 1_555 yes P2 RH P3 97.10(4) . 1_555 1_555 yes P2 RH SI 93.39(4) . 1_555 1_555 yes P3 RH SI 96.20(4) . 1_555 1_555 yes RH P1 C2 109.3(1) . 1_555 1_555 yes RH P1 C5 119.8(1) . 1_555 1_555 yes RH P1 C11 117.4(1) . 1_555 1_555 yes C2 P1 C5 104.1(2) . 1_555 1_555 yes C2 P1 C11 103.1(2) . 1_555 1_555 yes C5 P1 C11 101.1(2) . 1_555 1_555 yes RH P2 C17 116.3(2) . 1_555 1_555 yes RH P2 C18 110.8(2) . 1_555 1_555 yes RH P2 C19 123.1(2) . 1_555 1_555 yes C17 P2 C18 101.1(2) . 1_555 1_555 yes C17 P2 C19 101.2(2) . 1_555 1_555 yes C18 P2 C19 101.2(2) . 1_555 1_555 yes RH P3 C20 116.2(1) . 1_555 1_555 yes RH P3 C21 118.3(2) . 1_555 1_555 yes RH P3 C22 117.7(1) . 1_555 1_555 yes C20 P3 C21 100.7(2) . 1_555 1_555 yes C20 P3 C22 100.0(2) . 1_555 1_555 yes C21 P3 C22 100.7(2) . 1_555 1_555 yes RH SI C1 106.3(1) . 1_555 1_555 yes RH SI C3 120.7(2) . 1_555 1_555 yes RH SI C4 114.8(2) . 1_555 1_555 yes C1 SI C3 105.1(2) . 1_555 1_555 yes C1 SI C4 103.3(2) . 1_555 1_555 yes C3 SI C4 104.9(2) . 1_555 1_555 yes SI C1 C2 108.6(3) . 1_555 1_555 yes P1 C2 C1 108.5(3) . 1_555 1_555 yes P1 C5 C6 123.9(3) . 1_555 1_555 yes P1 C5 C10 117.9(3) . 1_555 1_555 yes C6 C5 C10 118.2(3) . 1_555 1_555 yes C5 C6 C7 120.4(4) . 1_555 1_555 yes C6 C7 C8 120.8(4) . 1_555 1_555 yes C7 C8 C9 119.6(4) . 1_555 1_555 yes C8 C9 C10 120.0(4) . 1_555 1_555 yes C5 C10 C9 121.0(4) . 1_555 1_555 yes P1 C11 C12 120.6(3) . 1_555 1_555 yes P1 C11 C16 120.4(3) . 1_555 1_555 yes C12 C11 C16 118.8(4) . 1_555 1_555 yes C11 C12 C13 120.3(4) . 1_555 1_555 yes C12 C13 C14 120.0(4) . 1_555 1_555 yes C13 C14 C15 120.4(4) . 1_555 1_555 yes C14 C15 C16 119.3(4) . 1_555 1_555 yes C11 C16 C15 121.1(4) . 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 CL 2.535(1) . . ? C9 C12 3.524(6) . 7_555 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_complex_2 _database_code_CSD 173811 _audit_creation_date 'Tue Nov 21 22:25:31 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C22 H38 P3 Rh Si ' _chemical_formula_moiety 'C22 H38 P3 Rh Si ' _chemical_formula_weight 526.45 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.4349(6) _cell_length_b 12.9113(9) _cell_length_c 9.5714(4) _cell_angle_alpha 100.379(5) _cell_angle_beta 104.093(2) _cell_angle_gamma 106.562(3) _cell_volume 1265.5(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6165 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _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 1.381 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details Coppens_numerical _exptl_absorpt_correction_T_min 0.644 _exptl_absorpt_correction_T_max 0.853 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11725 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9658 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9658 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # 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 5596 _reflns_number_gt 5481 _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 0.1893 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5596 _refine_ls_number_parameters 244 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.15000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.1793 _refine_diff_density_max 0.45 _refine_diff_density_min -0.94 _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) ; 'Si' 'Si' 0.082 0.070 ;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) ; '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 Rh 0.23457(2) 0.24182(1) 0.52378(2) 0.0130(1) Uani 1.00 d . . . P1 P 0.14809(6) 0.28059(6) 0.30838(7) 0.0152(2) Uani 1.00 d . . . P2 P 0.30417(6) 0.16394(6) 0.70930(8) 0.0167(2) Uani 1.00 d . . . P3 P 0.22559(7) 0.39684(6) 0.68361(9) 0.0178(2) Uani 1.00 d . . . Si Si 0.24639(8) 0.08963(7) 0.34999(9) 0.0183(2) Uani 1.00 d . . . C1 C 0.4146(3) 0.1161(3) 0.3342(4) 0.0337(9) Uani 1.00 d . . . C2 C 0.1867(3) -0.0652(2) 0.3495(4) 0.0298(8) Uani 1.00 d . . . C3 C 0.1509(3) 0.0836(3) 0.1536(3) 0.0237(7) Uani 1.00 d . . . C4 C 0.1753(3) 0.2038(3) 0.1448(3) 0.0256(7) Uani 1.00 d . . . C5 C -0.0275(2) 0.2435(2) 0.2510(3) 0.0181(6) Uani 1.00 d . . . C6 C -0.0905(3) 0.2329(2) 0.3578(3) 0.0201(6) Uani 1.00 d . . . C7 C -0.2227(3) 0.2083(2) 0.3208(4) 0.0270(7) Uani 1.00 d . . . C8 C -0.2953(3) 0.1915(3) 0.1749(4) 0.0313(8) Uani 1.00 d . . . C9 C -0.2353(3) 0.1985(3) 0.0654(4) 0.0362(9) Uani 1.00 d . . . C10 C -0.1023(3) 0.2242(3) 0.1032(3) 0.0283(7) Uani 1.00 d . . . C11 C 0.2063(2) 0.4248(2) 0.2911(3) 0.0188(6) Uani 1.00 d . . . C12 C 0.3379(3) 0.4845(3) 0.3552(4) 0.0297(8) Uani 1.00 d . . . C13 C 0.3918(3) 0.5933(3) 0.3502(5) 0.0403(9) Uani 1.00 d . . . C14 C 0.3122(3) 0.6450(3) 0.2805(5) 0.0411(10) Uani 1.00 d . . . C15 C 0.1823(3) 0.5884(3) 0.2150(4) 0.0354(9) Uani 1.00 d . . . C16 C 0.1286(3) 0.4786(3) 0.2214(3) 0.0237(7) Uani 1.00 d . . . C17 C 0.4067(3) 0.0785(3) 0.6985(4) 0.0257(7) Uani 1.00 d . . . C18 C 0.1680(3) 0.0676(3) 0.7443(4) 0.0276(7) Uani 1.00 d . . . C19 C 0.3993(3) 0.2524(3) 0.9013(3) 0.0282(7) Uani 1.00 d . . . C20 C 0.1391(3) 0.3657(3) 0.8184(4) 0.0319(8) Uani 1.00 d . . . C21 C 0.3785(3) 0.5043(3) 0.8059(4) 0.0401(9) Uani 1.00 d . . . C22 C 0.1476(3) 0.4910(3) 0.6141(4) 0.0300(8) Uani 1.00 d . . . H H 0.3488 0.7220 0.2790 0.0478 Uiso 1.00 d . . . H1 H 0.4136 0.0559 0.2599 0.0402 Uiso 1.00 calc . . . H2 H 0.4420 0.1842 0.3073 0.0402 Uiso 1.00 calc . . . H3 H 0.4720 0.1213 0.4277 0.0402 Uiso 1.00 calc . . . H4 H 0.2067 -0.1087 0.2738 0.0358 Uiso 1.00 calc . . . H5 H 0.0965 -0.0903 0.3311 0.0358 Uiso 1.00 calc . . . H6 H 0.2277 -0.0731 0.4443 0.0358 Uiso 1.00 calc . . . H7 H 0.1786 0.0445 0.0814 0.0287 Uiso 1.00 calc . . . H8 H 0.0618 0.0463 0.1356 0.0287 Uiso 1.00 calc . . . H9 H 0.1180 0.2053 0.0554 0.0309 Uiso 1.00 calc . . . H10 H 0.2614 0.2370 0.1463 0.0309 Uiso 1.00 calc . . . H11 H -0.0420 0.2430 0.4584 0.0238 Uiso 1.00 calc . . . H12 H -0.2641 0.2029 0.3957 0.0328 Uiso 1.00 calc . . . H13 H -0.3853 0.1752 0.1492 0.0377 Uiso 1.00 calc . . . H14 H -0.2849 0.1858 -0.0353 0.0427 Uiso 1.00 calc . . . H15 H -0.0623 0.2285 0.0270 0.0339 Uiso 1.00 calc . . . H16 H 0.3919 0.4491 0.4037 0.0355 Uiso 1.00 calc . . . H17 H 0.4815 0.6323 0.3935 0.0481 Uiso 1.00 calc . . . H18 H 0.3485 0.7210 0.2787 0.0490 Uiso 1.00 calc . . . H19 H 0.1293 0.6243 0.1661 0.0427 Uiso 1.00 calc . . . H20 H 0.0387 0.4401 0.1777 0.0283 Uiso 1.00 calc . . . H21 H 0.3739 0.0252 0.6036 0.0308 Uiso 1.00 calc . . . H22 H 0.4916 0.1256 0.7120 0.0308 Uiso 1.00 calc . . . H23 H 0.4078 0.0403 0.7748 0.0308 Uiso 1.00 calc . . . H24 H 0.1297 0.0011 0.6642 0.0329 Uiso 1.00 calc . . . H25 H 0.1978 0.0493 0.8352 0.0329 Uiso 1.00 calc . . . H26 H 0.1064 0.1027 0.7519 0.0329 Uiso 1.00 calc . . . H27 H 0.4017 0.2062 0.9681 0.0340 Uiso 1.00 calc . . . H28 H 0.3604 0.3051 0.9305 0.0340 Uiso 1.00 calc . . . H29 H 0.4841 0.2910 0.9036 0.0340 Uiso 1.00 calc . . . H30 H 0.0501 0.3310 0.7675 0.0383 Uiso 1.00 calc . . . H31 H 0.1698 0.3167 0.8687 0.0383 Uiso 1.00 calc . . . H32 H 0.1543 0.4335 0.8898 0.0383 Uiso 1.00 calc . . . H33 H 0.4334 0.4689 0.8527 0.0479 Uiso 1.00 calc . . . H34 H 0.3628 0.5532 0.8798 0.0479 Uiso 1.00 calc . . . H35 H 0.4188 0.5460 0.7476 0.0479 Uiso 1.00 calc . . . H36 H 0.1627 0.5533 0.6941 0.0360 Uiso 1.00 calc . . . H37 H 0.1819 0.5167 0.5403 0.0360 Uiso 1.00 calc . . . H38 H 0.0579 0.4519 0.5706 0.0360 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 0.0138(2) 0.0133(2) 0.0121(2) 0.0051(1) 0.0031(1) 0.0046(1) P1 0.0154(3) 0.0176(4) 0.0144(4) 0.0058(3) 0.0052(3) 0.0078(3) P2 0.0183(3) 0.0165(4) 0.0152(4) 0.0067(3) 0.0026(3) 0.0064(3) P3 0.0207(4) 0.0159(4) 0.0150(4) 0.0078(3) 0.0021(3) 0.0023(3) Si 0.0225(4) 0.0177(4) 0.0170(4) 0.0091(3) 0.0077(3) 0.0046(3) C1 0.031(2) 0.042(2) 0.039(2) 0.020(1) 0.020(1) 0.013(1) C2 0.036(2) 0.017(1) 0.033(2) 0.007(1) 0.007(1) 0.006(1) C3 0.031(1) 0.028(2) 0.012(1) 0.012(1) 0.006(1) 0.004(1) C4 0.034(1) 0.035(2) 0.017(1) 0.019(1) 0.012(1) 0.014(1) C5 0.019(1) 0.015(1) 0.016(1) 0.0038(9) 0.0003(9) 0.0054(9) C6 0.025(1) 0.017(1) 0.021(1) 0.0072(10) 0.0078(10) 0.0095(10) C7 0.026(1) 0.020(1) 0.039(2) 0.009(1) 0.012(1) 0.015(1) C8 0.017(1) 0.029(2) 0.045(2) 0.004(1) 0.004(1) 0.017(1) C9 0.022(1) 0.048(2) 0.031(2) 0.009(1) -0.007(1) 0.015(1) C10 0.021(1) 0.038(2) 0.021(1) 0.006(1) 0.003(1) 0.011(1) C11 0.022(1) 0.021(1) 0.018(1) 0.007(1) 0.0099(10) 0.0112(10) C12 0.021(1) 0.031(2) 0.039(2) 0.006(1) 0.008(1) 0.019(1) C13 0.029(2) 0.033(2) 0.056(2) 0.001(1) 0.014(1) 0.022(2) C14 0.037(2) 0.024(2) 0.071(3) 0.007(1) 0.025(2) 0.027(2) C15 0.031(2) 0.033(2) 0.056(2) 0.016(1) 0.020(1) 0.028(2) C16 0.018(1) 0.028(1) 0.030(2) 0.007(1) 0.009(1) 0.016(1) C17 0.024(1) 0.025(1) 0.034(2) 0.013(1) 0.007(1) 0.015(1) C18 0.030(1) 0.025(1) 0.032(2) 0.008(1) 0.016(1) 0.014(1) C19 0.032(1) 0.028(2) 0.018(1) 0.011(1) -0.003(1) 0.005(1) C20 0.038(2) 0.035(2) 0.033(2) 0.020(1) 0.020(1) 0.012(1) C21 0.036(2) 0.028(2) 0.039(2) 0.006(1) -0.004(1) -0.002(1) C22 0.040(2) 0.025(1) 0.029(2) 0.021(1) 0.006(1) 0.006(1) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF94 (PATTY)' _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 P1 2.2672(7) . . yes RH P2 2.2823(7) . . yes RH P3 2.3339(7) . . yes RH SI 2.3937(8) . . yes P1 C4 1.840(3) . . yes P1 C5 1.839(3) . . yes P1 C11 1.843(3) . . yes P2 C17 1.832(3) . . yes P2 C18 1.840(3) . . yes P2 C19 1.851(3) . . yes P3 C20 1.840(3) . . yes P3 C21 1.841(3) . . yes P3 C22 1.827(3) . . yes SI C1 1.903(3) . . yes SI C2 1.918(3) . . yes SI C3 1.906(3) . . yes C3 C4 1.519(4) . . yes C5 C6 1.391(4) . . yes C5 C10 1.399(4) . . yes C6 C7 1.391(4) . . yes C7 C8 1.383(4) . . yes C8 C9 1.387(5) . . yes C9 C10 1.399(4) . . yes C11 C12 1.398(4) . . yes C11 C16 1.396(4) . . yes C12 C13 1.379(4) . . yes C13 C14 1.389(5) . . yes C14 C15 1.376(5) . . yes C15 C16 1.394(4) . . 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 P1 RH P2 167.65(3) . 1_555 1_555 yes P1 RH P3 95.96(3) . 1_555 1_555 yes P1 RH SI 81.24(3) . 1_555 1_555 yes P2 RH P3 95.13(3) . 1_555 1_555 yes P2 RH SI 87.85(3) . 1_555 1_555 yes P3 RH SI 176.58(2) . 1_555 1_555 yes RH P1 C4 113.34(9) . 1_555 1_555 yes RH P1 C5 114.99(9) . 1_555 1_555 yes RH P1 C11 119.32(9) . 1_555 1_555 yes C4 P1 C5 103.2(1) . 1_555 1_555 yes C4 P1 C11 100.1(1) . 1_555 1_555 yes C5 P1 C11 103.7(1) . 1_555 1_555 yes RH P2 C17 123.2(1) . 1_555 1_555 yes RH P2 C18 111.07(10) . 1_555 1_555 yes RH P2 C19 121.0(1) . 1_555 1_555 yes C17 P2 C18 101.2(1) . 1_555 1_555 yes C17 P2 C19 95.5(1) . 1_555 1_555 yes C18 P2 C19 101.1(2) . 1_555 1_555 yes RH P3 C20 115.8(1) . 1_555 1_555 yes RH P3 C21 117.8(1) . 1_555 1_555 yes RH P3 C22 122.2(1) . 1_555 1_555 yes C20 P3 C21 101.8(2) . 1_555 1_555 yes C20 P3 C22 97.5(1) . 1_555 1_555 yes C21 P3 C22 97.8(2) . 1_555 1_555 yes RH SI C1 112.4(1) . 1_555 1_555 yes RH SI C2 125.4(1) . 1_555 1_555 yes RH SI C3 108.60(10) . 1_555 1_555 yes C1 SI C2 104.4(1) . 1_555 1_555 yes C1 SI C3 101.8(1) . 1_555 1_555 yes C2 SI C3 101.3(1) . 1_555 1_555 yes SI C3 C4 107.1(2) . 1_555 1_555 yes P1 C4 C3 107.6(2) . 1_555 1_555 yes P1 C5 C6 119.3(2) . 1_555 1_555 yes P1 C5 C10 123.0(2) . 1_555 1_555 yes C6 C5 C10 117.7(2) . 1_555 1_555 yes C5 C6 C7 121.5(3) . 1_555 1_555 yes C6 C7 C8 120.3(3) . 1_555 1_555 yes C7 C8 C9 119.4(3) . 1_555 1_555 yes C8 C9 C10 120.2(3) . 1_555 1_555 yes C5 C10 C9 120.9(3) . 1_555 1_555 yes P1 C11 C12 117.0(2) . 1_555 1_555 yes P1 C11 C16 124.8(2) . 1_555 1_555 yes C12 C11 C16 118.2(2) . 1_555 1_555 yes C11 C12 C13 121.9(3) . 1_555 1_555 yes C12 C13 C14 118.7(3) . 1_555 1_555 yes C13 C14 C15 120.9(3) . 1_555 1_555 yes C14 C15 C16 120.0(3) . 1_555 1_555 yes C11 C16 C15 120.3(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 #------------------------------------------------------------------------------ #===END data_complex_3 _database_code_CSD 173812 _audit_creation_date 'Tue May 30 15:00:49 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C25 H47 P4 Rh Si ' _chemical_formula_moiety 'C25 H47 P4 Rh Si ' _chemical_formula_weight 602.53 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pccn' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,z 1/2+x,-y,1/2-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z 1/2-x,y,1/2+z x,1/2-y,1/2+z _cell_length_a 11.8518(3) _cell_length_b 35.8507(8) _cell_length_c 14.0432(2) _cell_angle_alpha 89 _cell_angle_beta 89 _cell_angle_gamma 90 _cell_volume 5966.9(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 63989 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _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 1.341 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.920 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23536 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9663 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9663 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # 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 6620 _reflns_number_gt 4709 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1186 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6620 _refine_ls_number_parameters 280 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.09200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0210 _refine_diff_density_max 0.41 _refine_diff_density_min -0.89 _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 '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) ; 'Rh' 'Rh' -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.082 0.070 ;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) ; #------------------------------------------------------------------------------ # 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 Rh -0.01326(2) 0.142812(7) 0.02958(2) 0.01707(7) Uani 1.00 d . . . P1 P 0.05937(7) 0.10911(2) -0.09404(7) 0.0196(2) Uani 1.00 d . . . P2 P -0.20796(7) 0.14945(3) 0.03968(7) 0.0237(2) Uani 1.00 d . . . P3 P 0.07258(7) 0.18447(3) 0.13205(7) 0.0227(2) Uani 1.00 d . . . P4 P 0.01146(7) 0.09245(3) 0.13450(7) 0.0213(2) Uani 1.00 d . . . Si Si -0.00157(7) 0.19091(3) -0.08940(7) 0.0211(2) Uani 1.00 d . . . C1 C 0.1377(3) 0.2175(1) -0.1010(3) 0.0277(9) Uani 1.00 d . . . C2 C -0.1065(3) 0.2309(1) -0.1004(3) 0.033(1) Uani 1.00 d . . . C3 C -0.0024(3) 0.1665(1) -0.2098(3) 0.0253(9) Uani 1.00 d . . . C4 C 0.0889(3) 0.13671(10) -0.2027(3) 0.0247(9) Uani 1.00 d . . . C5 C 0.1959(3) 0.0853(1) -0.0739(3) 0.0261(9) Uani 1.00 d . . . C6 C 0.2883(3) 0.1082(1) -0.0511(3) 0.031(1) Uani 1.00 d . . . C7 C 0.3908(3) 0.0933(1) -0.0251(3) 0.043(1) Uani 1.00 d . . . C8 C 0.4038(4) 0.0547(2) -0.0178(3) 0.046(1) Uani 1.00 d . . . C9 C 0.3137(3) 0.0319(1) -0.0385(3) 0.038(1) Uani 1.00 d . . . C10 C 0.2100(3) 0.0468(1) -0.0680(3) 0.0297(10) Uani 1.00 d . . . C11 C -0.0245(3) 0.07151(10) -0.1518(3) 0.0242(9) Uani 1.00 d . . . C12 C -0.1337(3) 0.0642(1) -0.1182(3) 0.0268(9) Uani 1.00 d . . . C13 C -0.2017(3) 0.0382(1) -0.1633(3) 0.032(1) Uani 1.00 d . . . C14 C -0.1646(4) 0.0198(1) -0.2434(3) 0.038(1) Uani 1.00 d . . . C15 C -0.0567(4) 0.0267(1) -0.2774(3) 0.035(1) Uani 1.00 d . . . C16 C 0.0126(3) 0.0522(1) -0.2318(3) 0.0291(10) Uani 1.00 d . . . C17 C -0.2629(3) 0.1908(1) 0.1022(3) 0.037(1) Uani 1.00 d . . . C18 C -0.2964(3) 0.1143(1) 0.1011(3) 0.036(1) Uani 1.00 d . . . C19 C -0.2913(3) 0.1521(1) -0.0702(3) 0.037(1) Uani 1.00 d . . . C20 C 0.0263(3) 0.2336(1) 0.1332(3) 0.031(1) Uani 1.00 d . . . C21 C 0.2270(3) 0.1909(1) 0.1266(3) 0.032(1) Uani 1.00 d . . . C22 C 0.0602(3) 0.1777(1) 0.2617(3) 0.034(1) Uani 1.00 d . . . C23 C -0.0614(3) 0.0911(1) 0.2500(3) 0.031(1) Uani 1.00 d . . . C24 C 0.1570(3) 0.0834(1) 0.1747(3) 0.0271(10) Uani 1.00 d . . . C25 C -0.0279(3) 0.0453(1) 0.0964(3) 0.0295(10) Uani 1.00 d . . . H1 H 0.1988 0.2008 -0.1107 0.0340 Uiso 1.00 calc . . . H2 H 0.1344 0.2345 -0.1537 0.0340 Uiso 1.00 calc . . . H3 H 0.1519 0.2317 -0.0444 0.0340 Uiso 1.00 calc . . . H4 H -0.0930 0.2492 -0.0510 0.0402 Uiso 1.00 calc . . . H5 H -0.0966 0.2436 -0.1605 0.0402 Uiso 1.00 calc . . . H6 H -0.1814 0.2225 -0.0958 0.0402 Uiso 1.00 calc . . . H7 H -0.0745 0.1557 -0.2222 0.0309 Uiso 1.00 calc . . . H8 H 0.0140 0.1840 -0.2597 0.0309 Uiso 1.00 calc . . . H9 H 0.1619 0.1479 -0.1988 0.0310 Uiso 1.00 calc . . . H10 H 0.0874 0.1208 -0.2577 0.0310 Uiso 1.00 calc . . . H11 H 0.2801 0.1350 -0.0538 0.0377 Uiso 1.00 calc . . . H12 H 0.4539 0.1094 -0.0114 0.0487 Uiso 1.00 calc . . . H13 H 0.4747 0.0443 0.0019 0.0534 Uiso 1.00 calc . . . H14 H 0.3216 0.0052 -0.0328 0.0466 Uiso 1.00 calc . . . H15 H 0.1497 0.0304 -0.0853 0.0348 Uiso 1.00 calc . . . H16 H -0.1614 0.0773 -0.0626 0.0334 Uiso 1.00 calc . . . H17 H -0.2766 0.0330 -0.1388 0.0390 Uiso 1.00 calc . . . H18 H -0.2132 0.0022 -0.2755 0.0435 Uiso 1.00 calc . . . H19 H -0.0304 0.0143 -0.3334 0.0424 Uiso 1.00 calc . . . H20 H 0.0873 0.0562 -0.2556 0.0337 Uiso 1.00 calc . . . H21 H -0.2496 0.1883 0.1695 0.0433 Uiso 1.00 calc . . . H22 H -0.2262 0.2126 0.0803 0.0433 Uiso 1.00 calc . . . H23 H -0.3420 0.1930 0.0921 0.0433 Uiso 1.00 calc . . . H24 H -0.3740 0.1191 0.0913 0.0443 Uiso 1.00 calc . . . H25 H -0.2791 0.0897 0.0777 0.0443 Uiso 1.00 calc . . . H26 H -0.2812 0.1145 0.1683 0.0443 Uiso 1.00 calc . . . H27 H -0.3661 0.1597 -0.0567 0.0449 Uiso 1.00 calc . . . H28 H -0.2577 0.1697 -0.1131 0.0449 Uiso 1.00 calc . . . H29 H -0.2927 0.1283 -0.1008 0.0449 Uiso 1.00 calc . . . H30 H 0.0767 0.2484 0.1702 0.0374 Uiso 1.00 calc . . . H31 H 0.0257 0.2434 0.0693 0.0374 Uiso 1.00 calc . . . H32 H -0.0477 0.2358 0.1587 0.0374 Uiso 1.00 calc . . . H33 H 0.2642 0.1692 0.1494 0.0394 Uiso 1.00 calc . . . H34 H 0.2495 0.1948 0.0613 0.0394 Uiso 1.00 calc . . . H35 H 0.2490 0.2118 0.1628 0.0394 Uiso 1.00 calc . . . H36 H -0.0151 0.1817 0.2816 0.0411 Uiso 1.00 calc . . . H37 H 0.0819 0.1527 0.2778 0.0411 Uiso 1.00 calc . . . H38 H 0.1090 0.1945 0.2942 0.0411 Uiso 1.00 calc . . . H39 H -0.0502 0.1142 0.2830 0.0379 Uiso 1.00 calc . . . H40 H -0.1396 0.0872 0.2414 0.0379 Uiso 1.00 calc . . . H41 H -0.0311 0.0715 0.2884 0.0379 Uiso 1.00 calc . . . H42 H 0.1557 0.0654 0.2250 0.0338 Uiso 1.00 calc . . . H43 H 0.2004 0.0740 0.1235 0.0338 Uiso 1.00 calc . . . H44 H 0.1897 0.1058 0.1978 0.0338 Uiso 1.00 calc . . . H45 H -0.1075 0.0431 0.0935 0.0355 Uiso 1.00 calc . . . H46 H 0.0029 0.0405 0.0344 0.0355 Uiso 1.00 calc . . . H47 H 0.0015 0.0274 0.1397 0.0355 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 0.0182(1) 0.0161(1) 0.0169(1) -0.00114(8) -0.00020(9) -0.00040(10) P1 0.0226(4) 0.0188(4) 0.0174(5) -0.0006(3) 0.0009(3) -0.0008(3) P2 0.0192(4) 0.0260(5) 0.0259(5) -0.0004(3) 0.0001(3) 0.0003(4) P3 0.0256(4) 0.0203(5) 0.0223(5) -0.0029(3) -0.0026(3) -0.0032(4) P4 0.0244(4) 0.0199(5) 0.0195(5) -0.0014(3) -0.0005(3) 0.0021(4) Si 0.0233(4) 0.0187(5) 0.0212(5) 0.0005(3) -0.0005(3) 0.0032(4) C1 0.031(2) 0.023(2) 0.030(2) -0.003(1) -0.001(1) 0.006(2) C2 0.042(2) 0.026(2) 0.032(2) 0.001(1) 0.004(2) 0.007(2) C3 0.034(2) 0.024(2) 0.018(2) -0.001(1) -0.003(1) 0.004(1) C4 0.028(2) 0.024(2) 0.021(2) 0.000(1) 0.002(1) 0.001(1) C5 0.031(2) 0.031(2) 0.017(2) 0.004(1) 0.002(1) -0.002(1) C6 0.029(2) 0.037(2) 0.027(2) -0.004(1) 0.003(1) 0.002(2) C7 0.023(2) 0.069(3) 0.036(3) 0.000(2) 0.000(2) 0.004(2) C8 0.034(2) 0.071(3) 0.032(3) 0.024(2) -0.002(2) 0.004(2) C9 0.040(2) 0.043(3) 0.030(2) 0.023(2) 0.001(2) 0.003(2) C10 0.035(2) 0.031(2) 0.023(2) 0.006(1) 0.005(1) 0.000(2) C11 0.030(2) 0.020(2) 0.022(2) 0.000(1) -0.005(1) 0.001(1) C12 0.033(2) 0.022(2) 0.025(2) 0.000(1) -0.005(1) 0.000(2) C13 0.031(2) 0.026(2) 0.039(2) -0.004(1) -0.010(2) 0.005(2) C14 0.056(2) 0.020(2) 0.037(2) -0.007(2) -0.020(2) 0.000(2) C15 0.057(3) 0.025(2) 0.023(2) 0.002(2) -0.010(2) -0.003(2) C16 0.038(2) 0.025(2) 0.023(2) 0.001(1) -0.001(1) -0.001(2) C17 0.029(2) 0.037(2) 0.044(3) 0.007(1) 0.009(2) -0.004(2) C18 0.017(2) 0.041(2) 0.051(3) -0.009(1) 0.006(2) 0.010(2) C19 0.024(2) 0.048(3) 0.037(2) -0.004(2) -0.005(2) 0.002(2) C20 0.038(2) 0.021(2) 0.035(2) -0.002(1) -0.005(2) -0.004(2) C21 0.023(2) 0.036(2) 0.038(2) -0.008(1) -0.012(1) -0.002(2) C22 0.048(2) 0.031(2) 0.023(2) -0.006(2) 0.000(2) -0.006(2) C23 0.032(2) 0.037(2) 0.023(2) -0.002(1) 0.005(1) 0.004(2) C24 0.025(2) 0.029(2) 0.028(2) 0.002(1) -0.002(1) 0.003(2) C25 0.038(2) 0.019(2) 0.031(2) -0.003(1) -0.010(2) 0.003(2) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF94 (PATTY)' _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 P1 2.2836(9) . . yes RH P2 2.3241(8) . . yes RH P3 2.3099(9) . . yes RH P4 2.3488(9) . . yes RH SI 2.405(1) . . yes P1 C4 1.852(4) . . yes P1 C5 1.850(4) . . yes P1 C11 1.860(4) . . yes P2 C17 1.842(4) . . yes P2 C18 1.853(4) . . yes P2 C19 1.835(4) . . yes P3 C20 1.846(4) . . yes P3 C21 1.846(3) . . yes P3 C22 1.844(4) . . yes P4 C23 1.838(4) . . yes P4 C24 1.844(3) . . yes P4 C25 1.832(4) . . yes SI C1 1.913(4) . . yes SI C2 1.906(4) . . yes SI C3 1.904(4) . . yes C3 C4 1.522(5) . . yes C5 C6 1.406(5) . . yes C5 C10 1.396(5) . . yes C6 C7 1.376(5) . . yes C7 C8 1.399(7) . . yes C8 C9 1.375(7) . . yes C9 C10 1.403(5) . . yes C11 C12 1.403(5) . . yes C11 C16 1.391(6) . . yes C12 C13 1.387(5) . . yes C13 C14 1.375(6) . . yes C14 C15 1.386(7) . . yes C15 C16 1.387(5) . . 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 P1 RH P2 118.35(3) . 1_555 1_555 yes P1 RH P3 130.51(3) . 1_555 1_555 yes P1 RH P4 91.32(3) . 1_555 1_555 yes P1 RH SI 80.18(3) . 1_555 1_555 yes P2 RH P3 109.46(3) . 1_555 1_555 yes P2 RH P4 99.45(3) . 1_555 1_555 yes P2 RH SI 91.50(3) . 1_555 1_555 yes P3 RH P4 92.94(3) . 1_555 1_555 yes P3 RH SI 86.78(3) . 1_555 1_555 yes P4 RH SI 168.45(3) . 1_555 1_555 yes RH P1 C4 114.5(1) . 1_555 1_555 yes RH P1 C5 117.2(1) . 1_555 1_555 yes RH P1 C11 120.9(1) . 1_555 1_555 yes C4 P1 C5 101.9(2) . 1_555 1_555 yes C4 P1 C11 97.4(2) . 1_555 1_555 yes C5 P1 C11 101.5(2) . 1_555 1_555 yes RH P2 C17 117.5(1) . 1_555 1_555 yes RH P2 C18 121.4(1) . 1_555 1_555 yes RH P2 C19 119.2(1) . 1_555 1_555 yes C17 P2 C18 97.2(2) . 1_555 1_555 yes C17 P2 C19 99.7(2) . 1_555 1_555 yes C18 P2 C19 97.0(2) . 1_555 1_555 yes RH P3 C20 119.4(1) . 1_555 1_555 yes RH P3 C21 119.5(1) . 1_555 1_555 yes RH P3 C22 119.7(1) . 1_555 1_555 yes C20 P3 C21 100.1(2) . 1_555 1_555 yes C20 P3 C22 95.4(2) . 1_555 1_555 yes C21 P3 C22 97.8(2) . 1_555 1_555 yes RH P4 C23 121.0(1) . 1_555 1_555 yes RH P4 C24 116.3(1) . 1_555 1_555 yes RH P4 C25 119.6(1) . 1_555 1_555 yes C23 P4 C24 99.5(2) . 1_555 1_555 yes C23 P4 C25 96.6(2) . 1_555 1_555 yes C24 P4 C25 99.6(2) . 1_555 1_555 yes RH SI C1 117.8(1) . 1_555 1_555 yes RH SI C2 124.0(1) . 1_555 1_555 yes RH SI C3 106.6(1) . 1_555 1_555 yes C1 SI C2 100.4(2) . 1_555 1_555 yes C1 SI C3 99.1(2) . 1_555 1_555 yes C2 SI C3 105.7(2) . 1_555 1_555 yes SI C3 C4 105.1(2) . 1_555 1_555 yes P1 C4 C3 107.1(2) . 1_555 1_555 yes P1 C5 C6 116.6(3) . 1_555 1_555 yes P1 C5 C10 124.8(3) . 1_555 1_555 yes C6 C5 C10 118.1(3) . 1_555 1_555 yes C5 C6 C7 121.5(4) . 1_555 1_555 yes C6 C7 C8 120.1(4) . 1_555 1_555 yes C7 C8 C9 119.1(4) . 1_555 1_555 yes C8 C9 C10 121.1(4) . 1_555 1_555 yes C5 C10 C9 120.0(4) . 1_555 1_555 yes P1 C11 C12 118.8(3) . 1_555 1_555 yes P1 C11 C16 123.0(3) . 1_555 1_555 yes C12 C11 C16 118.0(3) . 1_555 1_555 yes C11 C12 C13 120.6(4) . 1_555 1_555 yes C12 C13 C14 120.6(4) . 1_555 1_555 yes C13 C14 C15 119.5(4) . 1_555 1_555 yes C14 C15 C16 120.3(4) . 1_555 1_555 yes C11 C16 C15 121.0(4) . 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 C1 C1 3.538(7) . 2_555 ? C9 C14 3.590(6) . 3_554 ? #------------------------------------------------------------------------------