# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1654 data_9/05308E_Cole-Hamilton #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jul 8 09:51:05 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 7.402(5) _cell_length_b 11.785(5) _cell_length_c 12.520(4) _cell_angle_alpha 90 _cell_angle_beta 96.01(4) _cell_angle_gamma 90 _cell_volume 1086.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 493.2 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 6.1 _cell_measurement_theta_max 12.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P n ' _symmetry_Int_Tables_number 7 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_meas ? _chemical_formula_weight 636.08 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H33 I2 O P2 Rh ' _chemical_formula_moiety 'C14 H33 I2 O P2 Rh ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 612.00 _exptl_absorpt_coefficient_mu 3.771 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.698 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 493.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.51 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 -2 1 0 -1 1 -2 -1 _diffrn_reflns_number 2787 _reflns_number_total 2598 _reflns_number_observed 2453 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 4.90 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00860 _diffrn_orient_matrix_UB_12 -0.03058 _diffrn_orient_matrix_UB_13 -0.07484 _diffrn_orient_matrix_UB_21 0.02220 _diffrn_orient_matrix_UB_22 0.07776 _diffrn_orient_matrix_UB_23 -0.02791 _diffrn_orient_matrix_UB_31 0.13374 _diffrn_orient_matrix_UB_32 -0.01478 _diffrn_orient_matrix_UB_33 0.00835 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh 0 2 -1.118 0.919 'International Tables' I 0 4 -0.474 1.812 'International Tables' P 0 4 0.102 0.094 'International Tables' O 0 2 0.011 0.006 'International Tables' C 0 28 0.003 0.002 'International Tables' H 0 66 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom I(1) 0.4822 0.21911(4) 0.9375 0.0354(1) Uij ? ? I(2) 0.46805(9) 0.36228(5) 0.64437(5) 0.0388(1) Uij ? ? Rh(1) 0.2346 0.24329(5) 0.7559 0.0236(1) Uij ? ? P(1) 0.1291(3) 0.4174(2) 0.8245(2) 0.0303(5) Uij ? ? P(2) 0.3422(3) 0.0737(2) 0.6792(2) 0.0291(5) Uij ? ? O(1) -0.032(1) 0.1057(6) 0.8577(6) 0.066(2) Uij ? ? C(1) 0.070(1) 0.1597(7) 0.8229(6) 0.037(2) Uij ? ? C(2) 0.025(1) 0.2562(7) 0.6287(7) 0.040(2) Uij ? ? C(3) -0.058(1) 0.3966(7) 0.9062(7) 0.040(2) Uij ? ? C(4) -0.007(1) 0.3399(8) 1.0139(7) 0.045(3) Uij ? ? C(5) 0.033(1) 0.5148(7) 0.7188(7) 0.046(3) Uij ? ? C(6) -0.032(2) 0.6295(9) 0.7558(9) 0.066(4) Uij ? ? C(7) 0.285(1) 0.5037(7) 0.9134(7) 0.044(3) Uij ? ? C(8) 0.442(2) 0.5599(9) 0.8654(9) 0.073(4) Uij ? ? C(9) 0.256(1) -0.0583(6) 0.7321(7) 0.038(2) Uij ? ? C(10) 0.326(1) -0.0877(8) 0.8464(8) 0.050(3) Uij ? ? C(11) 0.273(1) 0.0480(7) 0.5359(6) 0.040(2) Uij ? ? C(12) 0.339(1) 0.1314(8) 0.4556(7) 0.050(3) Uij ? ? C(13) 0.589(1) 0.0566(7) 0.6957(7) 0.037(2) Uij ? ? C(14) 0.665(1) -0.0481(8) 0.6472(7) 0.045(3) Uij ? ? H(1) 0.0392 0.3245 0.5902 0.0478 Uij ? ? H(2) -0.0892 0.2566 0.6569 0.0478 Uij ? ? H(3) 0.0310 0.1933 0.5818 0.0478 Uij ? ? H(4) 0.0778 0.3859 1.0563 0.0537 Uij ? ? H(5) -0.1083 0.4689 0.9191 0.0477 Uij ? ? H(6) -0.1472 0.3510 0.8666 0.0477 Uij ? ? H(7) -0.1132 0.3306 1.0499 0.0537 Uij ? ? H(8) 0.0449 0.2678 1.0030 0.0537 Uij ? ? H(9) -0.0676 0.4779 0.6802 0.0555 Uij ? ? H(10) 0.1239 0.5285 0.6721 0.0555 Uij ? ? H(11) -0.1247 0.6182 0.8019 0.0791 Uij ? ? H(12) -0.0792 0.6726 0.6952 0.0791 Uij ? ? H(13) 0.0667 0.6689 0.7935 0.0791 Uij ? ? H(14) 0.3356 0.4561 0.9701 0.0526 Uij ? ? H(15) 0.2159 0.5621 0.9419 0.0526 Uij ? ? H(16) 0.5167 0.5034 0.8386 0.0877 Uij ? ? H(17) 0.5113 0.6030 0.9192 0.0877 Uij ? ? H(18) 0.3959 0.6085 0.8085 0.0877 Uij ? ? H(19) 0.1273 -0.0525 0.7284 0.0454 Uij ? ? H(20) 0.2874 -0.1187 0.6873 0.0454 Uij ? ? H(21) 0.2965 -0.0283 0.8928 0.0597 Uij ? ? H(22) 0.2712 -0.1563 0.8665 0.0597 Uij ? ? H(23) 0.4540 -0.0970 0.8516 0.0597 Uij ? ? H(24) 0.3163 -0.0250 0.5191 0.0480 Uij ? ? H(25) 0.1440 0.0484 0.5261 0.0480 Uij ? ? H(26) 0.2952 0.2052 0.4691 0.0605 Uij ? ? H(27) 0.2953 0.1088 0.3848 0.0605 Uij ? ? H(28) 0.4682 0.1322 0.4628 0.0605 Uij ? ? H(29) 0.6397 0.1208 0.6641 0.0446 Uij ? ? H(30) 0.6266 0.0556 0.7706 0.0446 Uij ? ? H(31) 0.6308 -0.0487 0.5719 0.0543 Uij ? ? H(32) 0.7936 -0.0476 0.6607 0.0543 Uij ? ? H(33) 0.6183 -0.1139 0.6786 0.0543 Uij ? ? 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) 0.0377(3) 0.0364(3) 0.0313(3) 0.0032(2) -0.0006(2) -0.0018(2) I(2) 0.0462(3) 0.0333(3) 0.0397(3) -0.0101(3) 0.0178(2) 0.0015(2) Rh(1) 0.0245(3) 0.0230(3) 0.0239(3) -0.0016(2) 0.0046(2) -0.0006(2) P(1) 0.033(1) 0.0262(10) 0.0317(10) 0.0024(8) 0.0057(8) -0.0020(8) P(2) 0.0283(10) 0.027(1) 0.0314(10) -0.0010(8) 0.0032(8) -0.0065(8) O(1) 0.063(5) 0.063(5) 0.072(5) -0.009(4) 0.016(4) -0.002(4) C(1) 0.037(4) 0.035(4) 0.038(4) -0.001(4) 0.005(4) -0.003(4) C(2) 0.045(5) 0.034(4) 0.044(5) 0.005(4) 0.016(4) -0.001(4) C(3) 0.036(4) 0.037(5) 0.047(5) 0.006(4) 0.009(4) -0.004(4) C(4) 0.052(5) 0.044(5) 0.041(5) -0.001(4) 0.017(4) -0.004(4) C(5) 0.068(6) 0.036(5) 0.036(4) 0.011(5) 0.011(4) 0.004(4) C(6) 0.083(8) 0.041(6) 0.076(7) 0.019(6) 0.018(6) 0.013(5) C(7) 0.051(6) 0.032(5) 0.049(5) -0.001(4) 0.004(4) -0.009(4) C(8) 0.071(7) 0.073(8) 0.080(8) -0.032(6) 0.029(6) -0.048(7) C(9) 0.037(4) 0.025(4) 0.052(5) -0.002(3) 0.006(4) -0.006(3) C(10) 0.048(6) 0.043(5) 0.057(5) -0.004(4) 0.006(5) 0.004(5) C(11) 0.039(5) 0.041(5) 0.038(4) 0.002(4) -0.003(4) -0.012(4) C(12) 0.062(6) 0.058(6) 0.032(4) 0.002(5) 0.005(4) -0.013(4) C(13) 0.031(4) 0.036(5) 0.045(5) 0.000(3) 0.002(3) -0.001(4) C(14) 0.036(5) 0.050(6) 0.050(5) 0.011(4) 0.006(4) -0.012(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 4.80711 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2453 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0263 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0272 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 4.042 _refine_ls_shift/esd_max 0.0340 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.19 _refine_diff_density_max 1.29 #------------------------------------------------------------------------------ _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 I(1) Rh(1) 2.7823(7) ? ? yes I(2) Rh(1) 2.721(1) ? ? yes Rh(1) P(1) 2.387(2) ? ? yes Rh(1) P(2) 2.390(2) ? ? yes Rh(1) C(1) 1.836(9) ? ? yes Rh(1) C(2) 2.109(9) ? ? yes P(1) C(3) 1.823(9) ? ? yes P(1) C(5) 1.839(9) ? ? yes P(1) C(7) 1.828(8) ? ? yes P(2) C(9) 1.832(8) ? ? yes P(2) C(11) 1.839(8) ? ? yes P(2) C(13) 1.826(8) ? ? yes O(1) C(1) 1.113(10) ? ? yes C(3) C(4) 1.52(1) ? ? yes C(5) C(6) 1.52(1) ? ? yes C(7) C(8) 1.51(1) ? ? yes C(9) C(10) 1.51(1) ? ? yes C(11) C(12) 1.52(1) ? ? yes C(13) C(14) 1.51(1) ? ? 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 I(1) Rh(1) I(2) 94.18(4) ? ? ? yes I(1) Rh(1) P(1) 90.34(5) ? ? ? yes I(1) Rh(1) P(2) 91.36(5) ? ? ? yes I(1) Rh(1) C(1) 89.0(2) ? ? ? yes I(1) Rh(1) C(2) 173.8(2) ? ? ? yes I(2) Rh(1) P(1) 89.48(5) ? ? ? yes I(2) Rh(1) P(2) 88.22(5) ? ? ? yes I(2) Rh(1) C(1) 176.3(2) ? ? ? yes I(2) Rh(1) C(2) 91.8(2) ? ? ? yes P(1) Rh(1) P(2) 177.24(7) ? ? ? yes P(1) Rh(1) C(1) 92.2(3) ? ? ? yes P(1) Rh(1) C(2) 88.1(2) ? ? ? yes P(2) Rh(1) C(1) 90.0(3) ? ? ? yes P(2) Rh(1) C(2) 90.4(2) ? ? ? yes C(1) Rh(1) C(2) 85.0(3) ? ? ? yes Rh(1) P(1) C(3) 112.5(3) ? ? ? yes Rh(1) P(1) C(5) 113.2(3) ? ? ? yes Rh(1) P(1) C(7) 119.2(3) ? ? ? yes C(3) P(1) C(5) 103.2(4) ? ? ? yes C(3) P(1) C(7) 101.7(4) ? ? ? yes C(5) P(1) C(7) 105.2(4) ? ? ? yes Rh(1) P(2) C(9) 114.9(3) ? ? ? yes Rh(1) P(2) C(11) 117.3(3) ? ? ? yes Rh(1) P(2) C(13) 114.7(3) ? ? ? yes C(9) P(2) C(11) 98.1(4) ? ? ? yes C(9) P(2) C(13) 104.4(4) ? ? ? yes C(11) P(2) C(13) 105.4(4) ? ? ? yes Rh(1) C(1) O(1) 175.8(8) ? ? ? yes P(1) C(3) C(4) 115.2(6) ? ? ? yes P(1) C(5) C(6) 116.5(7) ? ? ? yes P(1) C(7) C(8) 117.6(7) ? ? ? yes P(2) C(9) C(10) 116.0(6) ? ? ? yes P(2) C(11) C(12) 117.5(6) ? ? ? yes P(2) C(13) C(14) 117.1(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;