data_irh4p2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H47 Ir P2' _chemical_formula_weight 589.76 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' 0.0000 0.0000 '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' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' _cell_length_a 11.5580(6) _cell_length_b 11.5580(6) _cell_length_c 9.5846(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1280.38(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5089 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 31.45 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 5.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.319 _exptl_absorpt_correction_T_max 0.531 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; Bruker SAINT (SADABS) result: Ratio of minimum to maximum apparent transmission: 0.600872 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15188 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 30.47 _reflns_number_total 3898 _reflns_number_gt 3467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+0.5200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(6) _refine_ls_number_reflns 3898 _refine_ls_number_parameters 138 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0181 _refine_ls_R_factor_gt 0.0149 _refine_ls_wR_factor_ref 0.0349 _refine_ls_wR_factor_gt 0.0338 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ir1 Ir 0.5000 0.0000 0.00003(4) 0.01079(3) Uani 1 2 d S . . H1 H 0.593(3) 0.095(3) -0.033(5) 0.062(10) Uiso 1 1 d . . . H2 H 0.550(3) 0.056(3) 0.134(5) 0.080(13) Uiso 1 1 d . . . P1 P 0.64701(4) -0.13136(4) -0.03234(5) 0.01236(8) Uani 1 1 d . . . C1 C 0.5000 0.0000 -0.2197(3) 0.0137(5) Uani 1 2 d S . . C2 C 0.59015(18) -0.05230(17) -0.2950(2) 0.0146(4) Uani 1 1 d . . . C3 C 0.58856(19) -0.05436(19) -0.4400(2) 0.0181(4) Uani 1 1 d . . . H3 H 0.6482 -0.0931 -0.4897 0.022 Uiso 1 1 calc R . . C4 C 0.5000 0.0000 -0.5122(8) 0.0212(9) Uani 1 2 d S . . H4 H 0.5000 0.0000 -0.6113 0.025 Uiso 1 2 calc SR . . C5 C 0.69119(18) -0.10167(19) -0.2137(2) 0.0163(4) Uani 1 1 d . . . H5A H 0.7562 -0.0459 -0.2143 0.020 Uiso 1 1 calc R . . H5B H 0.7179 -0.1741 -0.2583 0.020 Uiso 1 1 calc R . . C6 C 0.60187(16) -0.28818(15) -0.0336(2) 0.0167(4) Uani 1 1 d . . . C7 C 0.5209(2) -0.3051(2) -0.1592(3) 0.0214(5) Uani 1 1 d . . . H7A H 0.5644 -0.2936 -0.2459 0.032 Uiso 1 1 calc R . . H7B H 0.4576 -0.2488 -0.1544 0.032 Uiso 1 1 calc R . . H7C H 0.4890 -0.3836 -0.1575 0.032 Uiso 1 1 calc R . . C8 C 0.70162(19) -0.37528(18) -0.0478(3) 0.0242(5) Uani 1 1 d . . . H8A H 0.7510 -0.3711 0.0351 0.036 Uiso 1 1 calc R . . H8B H 0.7474 -0.3567 -0.1309 0.036 Uiso 1 1 calc R . . H8C H 0.6700 -0.4536 -0.0567 0.036 Uiso 1 1 calc R . . C9 C 0.5331(2) -0.3157(2) 0.0994(3) 0.0228(5) Uani 1 1 d . . . H9A H 0.5030 -0.3949 0.0940 0.034 Uiso 1 1 calc R . . H9B H 0.4684 -0.2613 0.1082 0.034 Uiso 1 1 calc R . . H9C H 0.5838 -0.3085 0.1808 0.034 Uiso 1 1 calc R . . C10 C 0.78405(18) -0.11212(18) 0.0714(2) 0.0169(4) Uani 1 1 d . . . C11 C 0.89094(16) -0.16299(18) -0.0020(3) 0.0239(4) Uani 1 1 d . . . H11A H 0.9013 -0.1252 -0.0927 0.036 Uiso 1 1 calc R . . H11B H 0.8800 -0.2463 -0.0158 0.036 Uiso 1 1 calc R . . H11C H 0.9596 -0.1499 0.0558 0.036 Uiso 1 1 calc R . . C12 C 0.7699(2) -0.1661(2) 0.2173(2) 0.0236(5) Uani 1 1 d . . . H12A H 0.8351 -0.1430 0.2764 0.035 Uiso 1 1 calc R . . H12B H 0.7682 -0.2506 0.2091 0.035 Uiso 1 1 calc R . . H12C H 0.6975 -0.1390 0.2592 0.035 Uiso 1 1 calc R . . C13 C 0.8061(2) 0.0174(2) 0.0920(3) 0.0217(5) Uani 1 1 d . . . H13A H 0.8780 0.0283 0.1446 0.032 Uiso 1 1 calc R . . H13B H 0.7415 0.0517 0.1437 0.032 Uiso 1 1 calc R . . H13C H 0.8130 0.0551 0.0008 0.032 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01323(5) 0.01147(5) 0.00767(4) 0.000 0.000 0.00097(3) P1 0.0135(2) 0.0121(2) 0.01153(19) -0.00049(18) 0.00042(18) 0.00082(17) C1 0.0168(13) 0.0127(13) 0.0116(13) 0.000 0.000 -0.0036(10) C2 0.0175(9) 0.0149(9) 0.0114(9) -0.0009(7) 0.0014(7) -0.0028(7) C3 0.0196(10) 0.0208(10) 0.0140(10) -0.0025(8) 0.0032(8) -0.0044(8) C4 0.0270(13) 0.0268(14) 0.010(2) 0.000 0.000 -0.0080(11) C5 0.0160(10) 0.0195(10) 0.0135(9) -0.0005(7) 0.0026(7) -0.0003(7) C6 0.0181(8) 0.0131(8) 0.0189(9) -0.0009(8) -0.0001(8) 0.0008(6) C7 0.0221(12) 0.0166(11) 0.0255(13) -0.0050(10) -0.0027(11) -0.0018(9) C8 0.0256(10) 0.0161(9) 0.0310(12) -0.0040(9) -0.0028(10) 0.0047(8) C9 0.0249(12) 0.0156(11) 0.0280(13) 0.0044(9) 0.0032(9) -0.0014(9) C10 0.0152(9) 0.0174(10) 0.0180(10) 0.0000(8) -0.0026(8) 0.0001(7) C11 0.0154(8) 0.0291(10) 0.0271(11) -0.0049(11) -0.0026(10) 0.0030(7) C12 0.0247(11) 0.0293(12) 0.0169(11) 0.0023(9) -0.0045(9) 0.0008(9) C13 0.0187(11) 0.0215(11) 0.0247(13) -0.0031(10) -0.0058(10) -0.0037(9) _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. Distance H1H2 1.7293 (0.0915) H2 - H2_$1 1.7378 (0.0625) H1 - H2 1.5672 (0.0322) Ir1 - H1 1.5503 (0.0468) Ir1 - H2 Angle H1A1 156.77 ( 3.27) H1 - Ir1 - H1_$1 67.79 ( 3.46) H2 - Ir1 - H2_$1 135.47 ( 2.46) H1 - Ir1 - H2_$1 67.75 ( 2.30) H1 - Ir1 - H2 78.39 ( 1.64) H1 - Ir1 - C1 146.10 ( 1.73) H2 - Ir1 - C1 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 8.250(0.154) x - 8.094(0.157) y + 0.000 z = 4.125(0.077) * 0.000 (0.000) C1 * 0.000 (0.000) Ir1 * 0.000 (0.000) H1 -0.039 (0.036) H2 2.276 (0.002) P1 Rms deviation of fitted atoms = 0.0000 ; 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 Ir1 C1 2.106(3) . ? Ir1 P1 2.2997(5) . ? Ir1 P1 2.2997(5) 2_655 ? Ir1 H1 1.57(3) . ? Ir1 H2 1.55(5) . ? P1 C5 1.844(2) . ? P1 C10 1.883(2) . ? P1 C6 1.8861(18) . ? C1 C2 1.405(3) 2_655 ? C1 C2 1.405(3) . ? C2 C3 1.390(3) . ? C2 C5 1.516(3) . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C3 1.386(5) 2_655 ? C4 H4 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C9 1.536(3) . ? C6 C8 1.537(3) . ? C6 C7 1.537(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C13 1.531(3) . ? C10 C11 1.538(3) . ? C10 C12 1.540(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 C1 Ir1 P1 82.248(16) . . ? C1 Ir1 P1 82.249(16) . 2_655 ? P1 Ir1 P1 164.50(3) . 2_655 ? C1 Ir1 H1 78.4(16) . . ? P1 Ir1 H1 85.9(11) . . ? P1 Ir1 H1 91.0(11) 2_655 . ? C1 Ir1 H2 146.1(17) . . ? P1 Ir1 H2 96.4(12) . . ? P1 Ir1 H2 96.5(12) 2_655 . ? H1 Ir1 H2 68(2) . . ? C5 P1 C10 104.04(9) . . ? C5 P1 C6 104.43(10) . . ? C10 P1 C6 110.47(9) . . ? C5 P1 Ir1 102.06(7) . . ? C10 P1 Ir1 118.18(7) . . ? C6 P1 Ir1 115.53(6) . . ? C2 C1 C2 118.1(3) 2_655 . ? C2 C1 Ir1 120.95(14) 2_655 . ? C2 C1 Ir1 120.95(14) . . ? C3 C2 C1 120.8(2) . . ? C3 C2 C5 121.20(19) . . ? C1 C2 C5 117.97(19) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C3 120.1(6) . 2_655 ? C3 C4 H4 119.9 . . ? C3 C4 H4 119.9 2_655 . ? C2 C5 P1 109.98(14) . . ? C2 C5 H5A 109.7 . . ? P1 C5 H5A 109.7 . . ? C2 C5 H5B 109.7 . . ? P1 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C9 C6 C8 109.03(19) . . ? C9 C6 C7 107.95(17) . . ? C8 C6 C7 107.73(19) . . ? C9 C6 P1 109.69(15) . . ? C8 C6 P1 115.00(14) . . ? C7 C6 P1 107.20(15) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C10 C11 107.38(18) . . ? C13 C10 C12 107.25(19) . . ? C11 C10 C12 110.20(18) . . ? C13 C10 P1 108.89(15) . . ? C11 C10 P1 112.90(15) . . ? C12 C10 P1 110.02(15) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C5 19.31(7) . . . . ? P1 Ir1 P1 C5 19.31(7) 2_655 . . . ? C1 Ir1 P1 C10 132.63(8) . . . . ? P1 Ir1 P1 C10 132.63(8) 2_655 . . . ? C1 Ir1 P1 C6 -93.30(8) . . . . ? P1 Ir1 P1 C6 -93.30(8) 2_655 . . . ? P1 Ir1 C1 C2 168.33(9) . . . 2_655 ? P1 Ir1 C1 C2 -11.67(9) 2_655 . . 2_655 ? P1 Ir1 C1 C2 -11.67(9) . . . . ? P1 Ir1 C1 C2 168.33(9) 2_655 . . . ? C2 C1 C2 C3 -1.43(14) 2_655 . . . ? Ir1 C1 C2 C3 178.57(14) . . . . ? C2 C1 C2 C5 176.05(19) 2_655 . . . ? Ir1 C1 C2 C5 -3.95(19) . . . . ? C1 C2 C3 C4 2.9(3) . . . . ? C5 C2 C3 C4 -174.52(16) . . . . ? C2 C3 C4 C3 -1.43(14) . . . 2_655 ? C3 C2 C5 P1 -160.68(17) . . . . ? C1 C2 C5 P1 21.9(2) . . . . ? C10 P1 C5 C2 -150.33(14) . . . . ? C6 P1 C5 C2 93.79(15) . . . . ? Ir1 P1 C5 C2 -26.88(15) . . . . ? C5 P1 C6 C9 -164.92(15) . . . . ? C10 P1 C6 C9 83.76(16) . . . . ? Ir1 P1 C6 C9 -53.71(17) . . . . ? C5 P1 C6 C8 71.78(19) . . . . ? C10 P1 C6 C8 -39.5(2) . . . . ? Ir1 P1 C6 C8 -177.00(15) . . . . ? C5 P1 C6 C7 -47.96(17) . . . . ? C10 P1 C6 C7 -159.27(15) . . . . ? Ir1 P1 C6 C7 63.26(16) . . . . ? C5 P1 C10 C13 78.36(17) . . . . ? C6 P1 C10 C13 -170.07(16) . . . . ? Ir1 P1 C10 C13 -33.87(18) . . . . ? C5 P1 C10 C11 -40.80(17) . . . . ? C6 P1 C10 C11 70.77(17) . . . . ? Ir1 P1 C10 C11 -153.02(13) . . . . ? C5 P1 C10 C12 -164.36(15) . . . . ? C6 P1 C10 C12 -52.79(17) . . . . ? Ir1 P1 C10 C12 83.41(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.639 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.058