# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1931 data_aug1599 _audit_creation_date 1999-08-20T10:14:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[In(P2C3tBu3)]' _chemical_formula_moiety 'C15 H27 In P2' _chemical_formula_structural 'C15 H27 In P2' _chemical_formula_sum 'C15 H27 In P2' _chemical_formula_weight 384.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.144(4) _cell_length_b 11.233(6) _cell_length_c 13.461(7) _cell_angle_alpha 112.48(4) _cell_angle_beta 93.13(5) _cell_angle_gamma 90.09(5) _cell_volume 856.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'thin plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.1 _exptl_absorpt_factor_muR 0.178 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.1925 _exptl_absorpt_correction_T_max 0.8368 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.90141E-1 _diffrn_orient_matrix_ub_12 -0.81393E-1 _diffrn_orient_matrix_ub_13 -0.26259E-1 _diffrn_orient_matrix_ub_21 -0.4153E-2 _diffrn_orient_matrix_ub_22 0.4462E-2 _diffrn_orient_matrix_ub_23 0.75406E-1 _diffrn_orient_matrix_ub_31 -0.135825 _diffrn_orient_matrix_ub_32 0.51207E-1 _diffrn_orient_matrix_ub_33 0.9472E-2 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_standards_decay_corr_max 1.043 _diffrn_standards_decay_corr_min 0.988 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 3 2 1 2 3 _diffrn_reflns_number 3022 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 3022 _reflns_number_gt 2082 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0005(16) _refine_ls_number_reflns 3022 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.117 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.184 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 In In 0.13711(12) 0.25832(7) 0.75282(6) 0.0300(3) Uani 1 1 d . . . P1 P -0.2715(4) 0.1200(2) 0.66045(18) 0.0226(6) Uani 1 1 d . A 1 P2 P -0.2574(4) 0.3382(2) 0.86921(18) 0.0240(6) Uani 1 1 d . A 1 C1 C -0.2714(13) 0.2767(8) 0.6527(6) 0.0177(18) Uani 1 1 d . A 1 C2 C -0.2670(14) 0.3814(8) 0.7552(7) 0.022(2) Uani 1 1 d . A 1 C3 C -0.2611(15) 0.1729(8) 0.7990(7) 0.0209(19) Uani 1 1 d . A 1 C4 C -0.2886(15) 0.2704(8) 0.5361(7) 0.0214(19) Uani 1 1 d . A 1 C5 C -0.2062(18) 0.1394(9) 0.4553(7) 0.035(3) Uani 1 1 d . A 1 H5A H -0.2228 0.1375 0.3819 0.052 Uiso 1 1 calc R A 1 H5B H -0.2921 0.0683 0.4599 0.052 Uiso 1 1 calc R A 1 H5C H -0.0522 0.1302 0.4735 0.052 Uiso 1 1 calc R A 1 C6 C -0.5241(16) 0.2752(10) 0.5026(8) 0.030(2) Uani 1 1 d . A 1 H6A H -0.5387 0.257 0.4253 0.045 Uiso 1 1 calc R A 1 H6B H -0.5791 0.3612 0.5428 0.045 Uiso 1 1 calc R A 1 H6C H -0.6084 0.2107 0.5179 0.045 Uiso 1 1 calc R A 1 C7 C -0.1526(18) 0.3703(10) 0.5131(8) 0.035(3) Uani 1 1 d . A 1 H7A H -0.2057 0.4567 0.5534 0.052 Uiso 1 1 calc R A 1 H7B H -0.1659 0.3526 0.4358 0.052 Uiso 1 1 calc R A 1 H7C H 0.0006 0.3656 0.5353 0.052 Uiso 1 1 calc R A 1 C8 C -0.2710(15) 0.5299(8) 0.7829(8) 0.025(2) Uani 1 1 d . A 1 C9 C -0.4473(17) 0.5680(10) 0.7178(9) 0.036(3) Uani 1 1 d . A 1 H9A H -0.4397 0.6615 0.7374 0.054 Uiso 1 1 calc R A 1 H9B H -0.5908 0.5432 0.7332 0.054 Uiso 1 1 calc R A 1 H9C H -0.4251 0.524 0.6408 0.054 Uiso 1 1 calc R A 1 C10 C -0.0465(16) 0.5807(9) 0.7703(8) 0.031(2) Uani 1 1 d . A 1 H10A H -0.0476 0.6749 0.796 0.047 Uiso 1 1 calc R A 1 H10B H -0.0132 0.5447 0.6943 0.047 Uiso 1 1 calc R A 1 H10C H 0.0648 0.555 0.8127 0.047 Uiso 1 1 calc R A 1 C11 C -0.3179(18) 0.6034(9) 0.9022(7) 0.032(2) Uani 1 1 d . A 1 H11A H -0.4638 0.5789 0.9149 0.048 Uiso 1 1 calc R A 1 H11B H -0.3104 0.6963 0.9192 0.048 Uiso 1 1 calc R A 1 H11C H -0.2092 0.5815 0.9481 0.048 Uiso 1 1 calc R A 1 C12 C -0.2665(15) 0.0766(8) 0.8560(7) 0.021(2) Uani 1 1 d . A 1 C13 C -0.1406(17) -0.0450(9) 0.7991(8) 0.034(2) Uani 1 1 d . A 1 H13A H -0.2021 -0.0882 0.725 0.05 Uiso 1 1 calc R A 1 H13B H -0.1516 -0.1031 0.8376 0.05 Uiso 1 1 calc R A 1 H13C H 0.013 -0.022 0.7981 0.05 Uiso 1 1 calc R A 1 C14 C -0.5031(17) 0.0394(10) 0.8586(8) 0.037(3) Uani 1 1 d . A 1 H14A H -0.5113 -0.0191 0.8969 0.055 Uiso 1 1 calc R A 1 H14B H -0.5658 -0.0038 0.7848 0.055 Uiso 1 1 calc R A 1 H14C H -0.585 0.117 0.8959 0.055 Uiso 1 1 calc R A 1 C15 C -0.1685(17) 0.1379(10) 0.9728(7) 0.032(2) Uani 1 1 d . A 1 H15A H -0.1786 0.0758 1.0075 0.049 Uiso 1 1 calc R A 1 H15B H -0.2494 0.215 1.0127 0.049 Uiso 1 1 calc R A 1 H15C H -0.0151 0.1619 0.9725 0.049 Uiso 1 1 calc R A 1 M1 C -0.2677(17) 0.2378(10) 0.7168(7) 0E1(10) Uiso 0 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In 0.0273(4) 0.0318(4) 0.0320(4) 0.0133(3) 0.0028(3) 0.0014(3) P1 0.0324(14) 0.0168(12) 0.0146(11) 0.0018(9) 0.0005(10) -0.0015(10) P2 0.0348(14) 0.0188(12) 0.0156(12) 0.0028(10) 0.0052(10) -0.0006(10) C1 0.017(4) 0.018(4) 0.012(4) 0.000(3) 0.001(3) 0.002(3) C2 0.024(5) 0.015(4) 0.024(5) 0.002(4) 0.008(4) -0.005(4) C3 0.026(5) 0.023(5) 0.012(4) 0.005(4) -0.001(4) -0.002(4) C4 0.030(5) 0.021(5) 0.014(4) 0.009(4) -0.001(4) 0.001(4) C5 0.053(7) 0.031(6) 0.016(5) 0.003(4) 0.012(5) 0.000(5) C6 0.031(5) 0.039(6) 0.021(5) 0.013(4) -0.011(4) -0.015(4) C7 0.043(6) 0.038(6) 0.020(5) 0.009(5) -0.001(5) -0.011(5) C8 0.027(5) 0.012(4) 0.032(5) 0.005(4) -0.001(4) -0.001(4) C9 0.042(6) 0.029(6) 0.040(6) 0.016(5) 0.012(5) 0.007(5) C10 0.033(6) 0.020(5) 0.039(6) 0.009(4) 0.004(5) -0.002(4) C11 0.047(6) 0.018(5) 0.024(5) 0.000(4) 0.004(5) 0.000(4) C12 0.033(5) 0.019(4) 0.010(4) 0.004(4) -0.002(4) -0.002(4) C13 0.042(6) 0.033(6) 0.029(5) 0.014(5) 0.007(5) 0.005(5) C14 0.040(6) 0.041(6) 0.033(6) 0.020(5) -0.002(5) -0.007(5) C15 0.041(6) 0.035(6) 0.020(5) 0.011(4) -0.007(4) -0.008(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In M1 2.501(11) . ? In C3 2.811(9) . ? In C1 2.829(9) . ? In C2 2.839(9) . ? In P1 2.904(3) . ? In P2 2.912(3) . ? P1 C3 1.725(9) . ? P1 C1 1.802(9) . ? P2 C3 1.730(9) . ? P2 C2 1.776(10) . ? C1 C2 1.429(11) . ? C1 C4 1.542(12) . ? C2 C8 1.564(12) . ? C3 C12 1.549(12) . ? C4 C6 1.499(13) . ? C4 C7 1.532(13) . ? C4 C5 1.563(12) . ? C8 C9 1.520(14) . ? C8 C10 1.535(12) . ? C8 C11 1.543(12) . ? C12 C14 1.518(13) . ? C12 C13 1.522(12) . ? C12 C15 1.542(13) . ? 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_3 _geom_angle_publ_flag M1 In C3 33.0(3) . . ? M1 In C1 22.9(3) . . ? C3 In C1 55.9(3) . . ? M1 In C2 31.7(3) . . ? C3 In C2 55.3(3) . . ? C1 In C2 29.2(2) . . ? M1 In P1 25.3(2) . . ? C3 In P1 35.08(18) . . ? C1 In P1 36.61(18) . . ? C2 In P1 56.45(18) . . ? M1 In P2 40.7(2) . . ? C3 In P2 35.14(18) . . ? C1 In P2 56.59(17) . . ? C2 In P2 35.95(18) . . ? P1 In P2 60.63(8) . . ? C3 P1 C1 97.0(4) . . ? C3 P1 In 69.5(3) . . ? C1 P1 In 69.4(3) . . ? C3 P2 C2 96.9(4) . . ? C3 P2 In 69.3(3) . . ? C2 P2 In 69.8(3) . . ? C2 C1 C4 132.8(8) . . ? C2 C1 P1 114.0(7) . . ? C4 C1 P1 113.1(6) . . ? C2 C1 In 75.8(5) . . ? C4 C1 In 120.7(5) . . ? P1 C1 In 74.0(3) . . ? C1 C2 C8 129.7(8) . . ? C1 C2 P2 115.8(7) . . ? C8 C2 P2 114.4(6) . . ? C1 C2 In 75.0(5) . . ? C8 C2 In 120.0(6) . . ? P2 C2 In 74.3(3) . . ? C12 C3 P1 121.2(6) . . ? C12 C3 P2 122.4(6) . . ? P1 C3 P2 116.3(5) . . ? C12 C3 In 120.9(6) . . ? P1 C3 In 75.4(3) . . ? P2 C3 In 75.6(3) . . ? C6 C4 C7 110.6(8) . . ? C6 C4 C1 108.9(7) . . ? C7 C4 C1 116.5(8) . . ? C6 C4 C5 105.6(8) . . ? C7 C4 C5 103.1(7) . . ? C1 C4 C5 111.5(7) . . ? C9 C8 C10 110.7(8) . . ? C9 C8 C11 106.0(8) . . ? C10 C8 C11 105.2(8) . . ? C9 C8 C2 113.2(8) . . ? C10 C8 C2 110.7(7) . . ? C11 C8 C2 110.6(8) . . ? C14 C12 C13 108.9(8) . . ? C14 C12 C15 108.4(7) . . ? C13 C12 C15 107.3(8) . . ? C14 C12 C3 107.9(8) . . ? C13 C12 C3 112.9(7) . . ? C15 C12 C3 111.3(7) . . ?