Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email stephan@uwindsor.ca _publ_contact_author_name 'Prof. Douglas Stephan' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name E.Hollink J.Stewart 'Pingrong Wei' D.W.Stephan data_m-C6H4(CH2P(t-Bu2))2 _database_code_CSD 215279 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H44 P2' _chemical_formula_weight 394.53 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 25.554(13) _cell_length_b 8.449(5) _cell_length_c 12.046(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.013(10) _cell_angle_gamma 90.00 _cell_volume 2597(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.344755 _exptl_absorpt_correction_T_max 0.488965 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 5318 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 23.24 _reflns_number_total 2921 _reflns_number_gt 2266 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0874P)^2^+0.2734P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(2) _refine_ls_number_reflns 2921 _refine_ls_number_parameters 235 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 1.707 _refine_ls_shift/su_mean 0.362 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 P1 P 0.48163(4) 0.1938(2) 0.61277(7) 0.0574(6) Uani 1 1 d . . . P2 P 0.70305(4) 0.1929(2) 0.40745(8) 0.0569(5) Uani 1 1 d . . . C1 C 0.5922(4) 0.3353(3) 0.5104(8) 0.0552(7) Uani 1 1 d . . . H1A H 0.5918 0.2252 0.5101 0.066 Uiso 1 1 calc R . . C2 C 0.5651(3) 0.4151(9) 0.5901(6) 0.0574(19) Uani 1 1 d . . . C3 C 0.5666(4) 0.5810(11) 0.5914(8) 0.089(3) Uani 1 1 d . . . H3A H 0.5501 0.6368 0.6462 0.107 Uiso 1 1 calc R . . C4 C 0.5925(5) 0.6610(4) 0.5113(12) 0.0937(16) Uani 1 1 d . . . H4A H 0.5920 0.7710 0.5096 0.112 Uiso 1 1 calc R . . C5 C 0.6198(3) 0.5766(10) 0.4323(6) 0.071(2) Uani 1 1 d . . . H5A H 0.6381 0.6321 0.3801 0.085 Uiso 1 1 calc R . . C6 C 0.6201(3) 0.4146(9) 0.4303(6) 0.061(2) Uani 1 1 d . . . C7 C 0.5352(3) 0.3208(9) 0.6711(6) 0.069(3) Uani 1 1 d . . . H7A H 0.5205 0.3939 0.7231 0.083 Uiso 1 1 calc R . . H7B H 0.5599 0.2540 0.7133 0.083 Uiso 1 1 calc R . . C8 C 0.4252(3) 0.3418(9) 0.5803(7) 0.067(2) Uani 1 1 d . . . C9 C 0.4404(3) 0.4202(9) 0.4761(5) 0.089(2) Uani 1 1 d . . . H9A H 0.4142 0.4965 0.4531 0.133 Uiso 1 1 calc R . . H9B H 0.4433 0.3421 0.4188 0.133 Uiso 1 1 calc R . . H9C H 0.4735 0.4725 0.4891 0.133 Uiso 1 1 calc R . . C10 C 0.3755(3) 0.2410(11) 0.5507(7) 0.102(3) Uani 1 1 d . . . H10A H 0.3462 0.3099 0.5340 0.153 Uiso 1 1 calc R . . H10B H 0.3681 0.1747 0.6127 0.153 Uiso 1 1 calc R . . H10C H 0.3814 0.1761 0.4871 0.153 Uiso 1 1 calc R . . C11 C 0.4132(4) 0.4626(10) 0.6711(7) 0.108(3) Uani 1 1 d . . . H11A H 0.3845 0.5288 0.6453 0.162 Uiso 1 1 calc R . . H11B H 0.4436 0.5269 0.6877 0.162 Uiso 1 1 calc R . . H11C H 0.4039 0.4076 0.7370 0.162 Uiso 1 1 calc R . . C12 C 0.4675(4) 0.0610(9) 0.7372(6) 0.069(2) Uani 1 1 d . . . C13 C 0.5164(4) -0.0355(10) 0.7549(10) 0.147(5) Uani 1 1 d . . . H13A H 0.5121 -0.1096 0.8142 0.221 Uiso 1 1 calc R . . H13B H 0.5455 0.0331 0.7740 0.221 Uiso 1 1 calc R . . H13C H 0.5230 -0.0920 0.6879 0.221 Uiso 1 1 calc R . . C14 C 0.4275(4) -0.0627(11) 0.7038(7) 0.107(3) Uani 1 1 d . . . H14A H 0.4205 -0.1269 0.7671 0.160 Uiso 1 1 calc R . . H14B H 0.4408 -0.1281 0.6465 0.160 Uiso 1 1 calc R . . H14C H 0.3958 -0.0121 0.6765 0.160 Uiso 1 1 calc R . . C15 C 0.4555(4) 0.1439(12) 0.8454(7) 0.121(4) Uani 1 1 d . . . H15A H 0.4469 0.0663 0.8998 0.182 Uiso 1 1 calc R . . H15B H 0.4263 0.2143 0.8322 0.182 Uiso 1 1 calc R . . H15C H 0.4855 0.2033 0.8723 0.182 Uiso 1 1 calc R . . C16 C 0.6502(3) 0.3249(9) 0.3423(7) 0.066(2) Uani 1 1 d . . . H16A H 0.6660 0.4007 0.2937 0.079 Uiso 1 1 calc R . . H16B H 0.6257 0.2609 0.2973 0.079 Uiso 1 1 calc R . . C17 C 0.7587(3) 0.3325(8) 0.4373(6) 0.064(2) Uani 1 1 d . . . C18 C 0.7707(5) 0.4454(10) 0.3463(9) 0.134(4) Uani 1 1 d . . . H18A H 0.7998 0.5110 0.3702 0.202 Uiso 1 1 calc R . . H18B H 0.7406 0.5107 0.3290 0.202 Uiso 1 1 calc R . . H18C H 0.7792 0.3871 0.2814 0.202 Uiso 1 1 calc R . . C19 C 0.7431(3) 0.4382(14) 0.5383(8) 0.174(5) Uani 1 1 d . . . H19A H 0.7707 0.5122 0.5566 0.261 Uiso 1 1 calc R . . H19B H 0.7376 0.3719 0.6014 0.261 Uiso 1 1 calc R . . H19C H 0.7114 0.4947 0.5183 0.261 Uiso 1 1 calc R . . C20 C 0.8090(4) 0.2499(12) 0.4753(9) 0.124(4) Uani 1 1 d . . . H20A H 0.8362 0.3271 0.4891 0.187 Uiso 1 1 calc R . . H20B H 0.8192 0.1780 0.4186 0.187 Uiso 1 1 calc R . . H20C H 0.8037 0.1921 0.5424 0.187 Uiso 1 1 calc R . . C21 C 0.7170(3) 0.0682(8) 0.2833(6) 0.066(2) Uani 1 1 d . . . C22 C 0.7639(4) -0.0422(11) 0.3134(9) 0.127(4) Uani 1 1 d . . . H22A H 0.7710 -0.1067 0.2504 0.191 Uiso 1 1 calc R . . H22B H 0.7555 -0.1088 0.3746 0.191 Uiso 1 1 calc R . . H22C H 0.7942 0.0204 0.3340 0.191 Uiso 1 1 calc R . . C23 C 0.7308(4) 0.1558(11) 0.1784(6) 0.103(3) Uani 1 1 d . . . H23A H 0.7358 0.0809 0.1201 0.154 Uiso 1 1 calc R . . H23B H 0.7624 0.2153 0.1929 0.154 Uiso 1 1 calc R . . H23C H 0.7027 0.2266 0.1562 0.154 Uiso 1 1 calc R . . C24 C 0.6661(4) -0.0274(10) 0.2481(8) 0.101(2) Uani 1 1 d . . . H24A H 0.6723 -0.0907 0.1840 0.151 Uiso 1 1 calc R . . H24B H 0.6379 0.0449 0.2307 0.151 Uiso 1 1 calc R . . H24C H 0.6569 -0.0950 0.3082 0.151 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 P1 0.0562(14) 0.0718(12) 0.0453(10) -0.0125(8) 0.0128(9) 0.0003(9) P2 0.0546(13) 0.0673(12) 0.0498(10) 0.0131(8) 0.0110(9) 0.0050(9) C1 0.0518(16) 0.0507(14) 0.0629(16) -0.001(5) 0.0022(13) 0.006(5) C2 0.042(5) 0.066(5) 0.063(5) -0.009(4) -0.005(4) 0.004(4) C3 0.065(6) 0.075(6) 0.126(7) -0.043(5) -0.016(5) -0.004(5) C4 0.077(2) 0.059(2) 0.143(4) 0.036(6) -0.022(3) -0.011(6) C5 0.061(6) 0.070(6) 0.082(5) 0.014(4) 0.005(4) -0.008(4) C6 0.049(5) 0.060(5) 0.073(5) 0.013(4) -0.001(4) 0.007(4) C7 0.068(6) 0.094(6) 0.048(4) -0.015(3) 0.016(4) 0.000(4) C8 0.047(4) 0.081(5) 0.071(4) 0.002(4) -0.019(3) 0.005(4) C9 0.093(6) 0.109(5) 0.061(4) 0.032(3) -0.019(4) -0.033(4) C10 0.047(5) 0.137(7) 0.121(7) 0.044(6) -0.014(4) -0.012(5) C11 0.145(9) 0.098(6) 0.078(5) -0.029(4) -0.009(5) 0.060(6) C12 0.069(5) 0.080(6) 0.059(4) 0.013(4) 0.021(4) 0.017(4) C13 0.135(9) 0.086(6) 0.225(12) 0.058(7) 0.057(8) 0.051(6) C14 0.115(7) 0.109(6) 0.094(5) 0.010(4) -0.006(5) -0.025(5) C15 0.172(11) 0.105(7) 0.088(6) 0.006(5) 0.022(6) 0.034(7) C16 0.053(5) 0.085(6) 0.060(5) 0.021(4) -0.005(4) 0.001(4) C17 0.078(6) 0.077(5) 0.039(3) -0.005(3) 0.017(3) 0.003(4) C18 0.172(9) 0.104(7) 0.124(7) 0.009(5) -0.032(7) -0.093(7) C19 0.070(6) 0.292(13) 0.159(8) -0.151(8) -0.005(5) -0.017(6) C20 0.074(7) 0.119(7) 0.179(10) 0.037(7) -0.003(6) 0.001(6) C21 0.066(5) 0.063(5) 0.070(4) 0.007(4) -0.002(4) -0.007(4) C22 0.120(8) 0.128(7) 0.134(8) -0.049(6) 0.007(6) 0.051(6) C23 0.151(9) 0.120(7) 0.040(4) -0.029(4) 0.035(5) -0.028(6) C24 0.083(5) 0.102(6) 0.118(5) -0.023(4) 0.009(4) -0.024(4) _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 P1 C7 1.849(8) . ? P1 C8 1.933(7) . ? P1 C12 1.922(7) . ? P2 C17 1.868(8) . ? P2 C21 1.879(8) . ? P2 C16 1.890(7) . ? C1 C2 1.388(10) . ? C1 C6 1.401(10) . ? C2 C7 1.500(10) . ? C2 C3 1.402(10) . ? C3 C4 1.376(13) . ? C4 C5 1.403(12) . ? C5 C6 1.369(10) . ? C6 C16 1.540(10) . ? C8 C9 1.489(10) . ? C8 C11 1.539(11) . ? C8 C10 1.556(11) . ? C12 C14 1.502(12) . ? C12 C13 1.498(12) . ? C12 C15 1.525(11) . ? C17 C20 1.513(13) . ? C17 C18 1.497(11) . ? C17 C19 1.577(10) . ? C21 C23 1.521(11) . ? C21 C24 1.571(12) . ? C21 C22 1.546(12) . ? 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 C7 P1 C8 103.4(3) . . ? C7 P1 C12 102.0(4) . . ? C8 P1 C12 111.5(4) . . ? C17 P2 C21 109.4(4) . . ? C17 P2 C16 103.2(3) . . ? C21 P2 C16 99.3(4) . . ? C2 C1 C6 122.4(2) . . ? C1 C2 C7 118.8(6) . . ? C1 C2 C3 118.6(7) . . ? C7 C2 C3 122.6(7) . . ? C4 C3 C2 119.8(8) . . ? C3 C4 C5 120.0(3) . . ? C6 C5 C4 121.6(7) . . ? C5 C6 C1 117.5(7) . . ? C5 C6 C16 120.5(7) . . ? C1 C6 C16 122.0(6) . . ? C2 C7 P1 116.9(5) . . ? C9 C8 C11 112.0(7) . . ? C9 C8 C10 107.2(6) . . ? C11 C8 C10 109.5(7) . . ? C9 C8 P1 103.5(6) . . ? C11 C8 P1 117.4(5) . . ? C10 C8 P1 106.5(5) . . ? C14 C12 C13 102.1(8) . . ? C14 C12 C15 112.5(7) . . ? C13 C12 C15 109.5(9) . . ? C14 C12 P1 110.5(6) . . ? C13 C12 P1 103.9(6) . . ? C15 C12 P1 117.0(6) . . ? C6 C16 P2 112.1(5) . . ? C20 C17 C18 108.2(8) . . ? C20 C17 C19 105.9(7) . . ? C18 C17 C19 105.9(7) . . ? C20 C17 P2 113.2(6) . . ? C18 C17 P2 116.4(6) . . ? C19 C17 P2 106.5(5) . . ? C23 C21 C24 104.5(7) . . ? C23 C21 C22 106.2(8) . . ? C24 C21 C22 111.9(7) . . ? C23 C21 P2 116.8(6) . . ? C24 C21 P2 108.3(6) . . ? C22 C21 P2 109.2(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.179 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.037 #===end data_m-C6H4(CH2(t-Bu2)PNSiMe3)2 _database_code_CSD 215280 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H62 N2 P2 Si2' _chemical_formula_weight 568.94 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.860(9) _cell_length_b 14.083(12) _cell_length_c 14.838(13) _cell_angle_alpha 65.975(16) _cell_angle_beta 75.781(16) _cell_angle_gamma 84.345(16) _cell_volume 1824(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.653759 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 7834 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.66 _reflns_number_total 5226 _reflns_number_gt 3816 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0903P)^2^+0.0000P] 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_number_reflns 5226 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.000 _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 P1 P 0.13708(7) 0.24129(5) 0.72688(5) 0.0371(2) Uani 1 1 d . . . P2 P 0.48939(6) 0.24631(5) 0.24222(5) 0.03415(19) Uani 1 1 d . . . Si1 Si -0.17924(8) 0.20802(7) 0.73282(7) 0.0520(2) Uani 1 1 d . . . Si2 Si 0.16915(7) 0.27927(6) 0.22839(6) 0.0443(2) Uani 1 1 d . . . N1 N -0.0100(2) 0.21043(18) 0.73021(18) 0.0509(6) Uani 1 1 d . . . N2 N 0.3339(2) 0.26023(17) 0.24072(18) 0.0477(6) Uani 1 1 d . . . C1 C -0.2706(4) 0.1043(3) 0.8526(3) 0.0835(11) Uani 1 1 d . . . H1A H -0.2575 0.1159 0.9094 0.125 Uiso 1 1 calc R . . H1B H -0.2327 0.0377 0.8560 0.125 Uiso 1 1 calc R . . H1C H -0.3687 0.1057 0.8543 0.125 Uiso 1 1 calc R . . C2 C -0.2716(4) 0.3335(3) 0.7252(4) 0.0968(13) Uani 1 1 d . . . H2A H -0.2596 0.3503 0.7793 0.145 Uiso 1 1 calc R . . H2B H -0.3695 0.3262 0.7309 0.145 Uiso 1 1 calc R . . H2C H -0.2329 0.3882 0.6613 0.145 Uiso 1 1 calc R . . C3 C -0.2092(4) 0.1790(4) 0.6261(3) 0.1075(15) Uani 1 1 d . . . H3A H -0.1637 0.2310 0.5625 0.161 Uiso 1 1 calc R . . H3B H -0.3077 0.1794 0.6297 0.161 Uiso 1 1 calc R . . H3C H -0.1713 0.1119 0.6316 0.161 Uiso 1 1 calc R . . C4 C 0.2911(4) 0.2705(4) 0.8558(3) 0.0961(14) Uani 1 1 d . . . H4A H 0.2892 0.2650 0.9227 0.144 Uiso 1 1 calc R . . H4B H 0.3081 0.3414 0.8087 0.144 Uiso 1 1 calc R . . H4C H 0.3642 0.2272 0.8371 0.144 Uiso 1 1 calc R . . C5 C 0.0337(4) 0.3012(3) 0.8897(3) 0.0807(11) Uani 1 1 d . . . H5A H 0.0409 0.2981 0.9542 0.121 Uiso 1 1 calc R . . H5B H -0.0560 0.2751 0.8960 0.121 Uiso 1 1 calc R . . H5C H 0.0437 0.3720 0.8412 0.121 Uiso 1 1 calc R . . C6 C 0.1213(5) 0.1217(3) 0.9292(2) 0.0898(12) Uani 1 1 d . . . H6A H 0.1274 0.1149 0.9951 0.135 Uiso 1 1 calc R . . H6B H 0.1895 0.0774 0.9072 0.135 Uiso 1 1 calc R . . H6C H 0.0294 0.1018 0.9322 0.135 Uiso 1 1 calc R . . C7 C 0.1494(3) 0.2349(2) 0.8540(2) 0.0528(7) Uani 1 1 d . . . C8 C 0.1186(4) 0.4598(2) 0.6456(3) 0.0696(9) Uani 1 1 d . . . H8A H 0.1513 0.5245 0.5908 0.104 Uiso 1 1 calc R . . H8B H 0.1365 0.4582 0.7070 0.104 Uiso 1 1 calc R . . H8C H 0.0199 0.4533 0.6538 0.104 Uiso 1 1 calc R . . C9 C 0.1531(4) 0.3687(2) 0.5289(2) 0.0605(8) Uani 1 1 d . . . H9A H 0.1813 0.4330 0.4720 0.091 Uiso 1 1 calc R . . H9B H 0.0534 0.3611 0.5434 0.091 Uiso 1 1 calc R . . H9C H 0.1980 0.3118 0.5134 0.091 Uiso 1 1 calc R . . C10 C 0.3549(3) 0.3868(2) 0.5945(3) 0.0692(9) Uani 1 1 d . . . H10A H 0.3774 0.4539 0.5404 0.104 Uiso 1 1 calc R . . H10B H 0.4021 0.3339 0.5734 0.104 Uiso 1 1 calc R . . H10C H 0.3846 0.3839 0.6526 0.104 Uiso 1 1 calc R . . C11 C 0.1958(3) 0.3691(2) 0.6222(2) 0.0464(7) Uani 1 1 d . . . C12 C 0.2711(3) 0.1464(2) 0.7059(2) 0.0420(6) Uani 1 1 d . . . H12A H 0.3619 0.1734 0.6981 0.050 Uiso 1 1 calc R . . H12B H 0.2561 0.0828 0.7667 0.050 Uiso 1 1 calc R . . C13 C 0.2780(2) 0.11817(18) 0.61637(19) 0.0366(6) Uani 1 1 d . . . C14 C 0.1711(3) 0.05996(19) 0.6173(2) 0.0426(6) Uani 1 1 d . . . H14A H 0.0937 0.0410 0.6716 0.051 Uiso 1 1 calc R . . C15 C 0.1793(3) 0.0300(2) 0.5378(2) 0.0473(7) Uani 1 1 d . . . H15A H 0.1080 -0.0097 0.5396 0.057 Uiso 1 1 calc R . . C16 C 0.2927(3) 0.05884(19) 0.4560(2) 0.0452(7) Uani 1 1 d . . . H16A H 0.2966 0.0388 0.4030 0.054 Uiso 1 1 calc R . . C17 C 0.4008(3) 0.11757(18) 0.45230(19) 0.0370(6) Uani 1 1 d . . . C18 C 0.3925(3) 0.14476(18) 0.53400(18) 0.0371(6) Uani 1 1 d . . . H18A H 0.4659 0.1819 0.5335 0.044 Uiso 1 1 calc R . . C19 C 0.5257(3) 0.1474(2) 0.36311(19) 0.0414(6) Uani 1 1 d . . . H19A H 0.5615 0.0853 0.3524 0.050 Uiso 1 1 calc R . . H19B H 0.5986 0.1740 0.3802 0.050 Uiso 1 1 calc R . . C20 C 0.5865(3) 0.1965(2) 0.1448(2) 0.0469(7) Uani 1 1 d . . . C21 C 0.5792(4) 0.2770(3) 0.0382(2) 0.0794(11) Uani 1 1 d . . . H21A H 0.6291 0.2513 -0.0115 0.119 Uiso 1 1 calc R . . H21B H 0.6206 0.3412 0.0264 0.119 Uiso 1 1 calc R . . H21C H 0.4832 0.2888 0.0334 0.119 Uiso 1 1 calc R . . C22 C 0.5080(3) 0.0984(3) 0.1647(3) 0.0696(9) Uani 1 1 d . . . H22A H 0.5536 0.0697 0.1165 0.104 Uiso 1 1 calc R . . H22B H 0.4133 0.1162 0.1582 0.104 Uiso 1 1 calc R . . H22C H 0.5079 0.0481 0.2320 0.104 Uiso 1 1 calc R . . C23 C 0.7399(3) 0.1668(3) 0.1487(2) 0.0636(8) Uani 1 1 d . . . H23A H 0.7815 0.1426 0.0962 0.095 Uiso 1 1 calc R . . H23B H 0.7438 0.1127 0.2134 0.095 Uiso 1 1 calc R . . H23C H 0.7903 0.2265 0.1387 0.095 Uiso 1 1 calc R . . C24 C 0.4981(4) 0.3876(3) 0.3238(3) 0.0801(11) Uani 1 1 d . . . H24A H 0.5345 0.4505 0.3196 0.120 Uiso 1 1 calc R . . H24B H 0.5190 0.3300 0.3815 0.120 Uiso 1 1 calc R . . H24C H 0.3986 0.3936 0.3308 0.120 Uiso 1 1 calc R . . C25 C 0.5216(4) 0.4616(2) 0.1390(3) 0.0750(10) Uani 1 1 d . . . H25A H 0.5610 0.5249 0.1313 0.113 Uiso 1 1 calc R . . H25B H 0.4214 0.4670 0.1525 0.113 Uiso 1 1 calc R . . H25C H 0.5551 0.4500 0.0779 0.113 Uiso 1 1 calc R . . C26 C 0.7258(3) 0.3707(3) 0.2106(4) 0.0899(12) Uani 1 1 d . . . H26A H 0.7557 0.4367 0.2035 0.135 Uiso 1 1 calc R . . H26B H 0.7673 0.3595 0.1500 0.135 Uiso 1 1 calc R . . H26C H 0.7543 0.3164 0.2673 0.135 Uiso 1 1 calc R . . C27 C 0.5652(3) 0.3699(2) 0.2280(2) 0.0449(7) Uani 1 1 d . . . C28 C 0.1029(4) 0.1678(3) 0.2134(3) 0.0891(12) Uani 1 1 d . . . H28A H 0.1120 0.1045 0.2701 0.134 Uiso 1 1 calc R . . H28B H 0.1564 0.1627 0.1520 0.134 Uiso 1 1 calc R . . H28C H 0.0062 0.1789 0.2103 0.134 Uiso 1 1 calc R . . C29 C 0.0519(4) 0.2905(4) 0.3420(3) 0.0938(13) Uani 1 1 d . . . H29A H 0.0813 0.3479 0.3518 0.141 Uiso 1 1 calc R . . H29B H 0.0558 0.2275 0.4003 0.141 Uiso 1 1 calc R . . H29C H -0.0423 0.3019 0.3328 0.141 Uiso 1 1 calc R . . C30 C 0.1481(4) 0.3988(3) 0.1154(3) 0.1010(14) Uani 1 1 d . . . H30A H 0.1791 0.4583 0.1209 0.151 Uiso 1 1 calc R . . H30B H 0.0513 0.4071 0.1122 0.151 Uiso 1 1 calc R . . H30C H 0.2029 0.3923 0.0551 0.151 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 P1 0.0384(4) 0.0371(4) 0.0389(4) -0.0164(3) -0.0116(3) -0.0007(3) P2 0.0312(4) 0.0335(4) 0.0385(4) -0.0127(3) -0.0126(3) 0.0016(3) Si1 0.0388(4) 0.0551(5) 0.0626(5) -0.0224(4) -0.0129(4) -0.0027(4) Si2 0.0341(4) 0.0530(5) 0.0485(4) -0.0186(4) -0.0185(3) 0.0042(3) N1 0.0371(13) 0.0563(15) 0.0665(16) -0.0303(13) -0.0122(12) -0.0047(11) N2 0.0351(13) 0.0433(13) 0.0643(15) -0.0164(12) -0.0206(11) 0.0037(10) C1 0.070(2) 0.065(2) 0.102(3) -0.024(2) -0.005(2) -0.0160(19) C2 0.062(2) 0.070(2) 0.136(4) -0.021(3) -0.024(2) 0.015(2) C3 0.079(3) 0.168(5) 0.109(3) -0.075(3) -0.040(3) -0.012(3) C4 0.080(3) 0.163(4) 0.077(3) -0.071(3) -0.029(2) -0.012(3) C5 0.091(3) 0.099(3) 0.063(2) -0.051(2) -0.008(2) 0.010(2) C6 0.141(4) 0.078(3) 0.0394(18) -0.0143(18) -0.019(2) 0.001(2) C7 0.0593(18) 0.0625(19) 0.0457(16) -0.0278(15) -0.0168(15) -0.0003(15) C8 0.091(3) 0.0396(17) 0.077(2) -0.0215(17) -0.021(2) 0.0036(17) C9 0.081(2) 0.0473(18) 0.0477(17) -0.0090(14) -0.0239(17) 0.0059(16) C10 0.066(2) 0.0547(19) 0.077(2) -0.0140(17) -0.0106(18) -0.0204(16) C11 0.0514(17) 0.0340(15) 0.0506(16) -0.0127(13) -0.0124(14) -0.0013(13) C12 0.0433(15) 0.0396(15) 0.0416(15) -0.0131(12) -0.0128(13) 0.0017(12) C13 0.0382(15) 0.0287(13) 0.0399(14) -0.0091(11) -0.0130(12) 0.0045(11) C14 0.0394(15) 0.0395(15) 0.0435(15) -0.0123(12) -0.0058(12) -0.0039(12) C15 0.0460(16) 0.0436(16) 0.0541(17) -0.0170(14) -0.0146(15) -0.0098(13) C16 0.0564(18) 0.0384(15) 0.0458(16) -0.0178(13) -0.0185(15) 0.0004(13) C17 0.0404(15) 0.0287(13) 0.0392(14) -0.0091(11) -0.0138(12) 0.0054(11) C18 0.0386(15) 0.0308(14) 0.0430(15) -0.0115(12) -0.0175(13) 0.0019(11) C19 0.0400(15) 0.0405(15) 0.0420(15) -0.0140(13) -0.0135(13) 0.0080(12) C20 0.0508(16) 0.0484(17) 0.0430(16) -0.0200(14) -0.0131(13) 0.0084(13) C21 0.110(3) 0.082(2) 0.0469(19) -0.0265(18) -0.027(2) 0.027(2) C22 0.071(2) 0.069(2) 0.087(2) -0.049(2) -0.0170(19) 0.0026(18) C23 0.0511(18) 0.070(2) 0.0602(19) -0.0255(17) -0.0020(16) 0.0112(16) C24 0.120(3) 0.053(2) 0.072(2) -0.0333(18) -0.007(2) -0.021(2) C25 0.100(3) 0.0436(18) 0.074(2) -0.0047(16) -0.033(2) -0.0154(18) C26 0.060(2) 0.084(3) 0.140(4) -0.047(3) -0.035(2) -0.0197(19) C27 0.0459(16) 0.0390(15) 0.0527(16) -0.0158(13) -0.0174(14) -0.0075(12) C28 0.067(2) 0.097(3) 0.128(3) -0.055(3) -0.044(2) -0.007(2) C29 0.062(2) 0.154(4) 0.088(3) -0.070(3) -0.031(2) 0.039(2) C30 0.072(2) 0.098(3) 0.101(3) 0.006(2) -0.046(2) 0.011(2) _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 P1 N1 1.538(2) . ? P1 C12 1.849(3) . ? P1 C11 1.864(3) . ? P1 C7 1.886(3) . ? P2 N2 1.531(2) . ? P2 C19 1.862(3) . ? P2 C20 1.873(3) . ? P2 C27 1.874(3) . ? Si1 N1 1.663(3) . ? Si1 C1 1.861(4) . ? Si1 C2 1.880(4) . ? Si1 C3 1.882(4) . ? Si2 N2 1.662(3) . ? Si2 C29 1.851(4) . ? Si2 C30 1.868(4) . ? Si2 C28 1.871(4) . ? C4 C7 1.540(4) . ? C5 C7 1.533(4) . ? C6 C7 1.533(5) . ? C8 C11 1.541(4) . ? C9 C11 1.544(4) . ? C10 C11 1.540(4) . ? C12 C13 1.519(4) . ? C13 C14 1.391(3) . ? C13 C18 1.394(4) . ? C14 C15 1.389(4) . ? C15 C16 1.381(4) . ? C16 C17 1.390(4) . ? C17 C18 1.395(3) . ? C17 C19 1.514(4) . ? C20 C23 1.538(4) . ? C20 C22 1.537(4) . ? C20 C21 1.540(4) . ? C24 C27 1.522(4) . ? C25 C27 1.542(4) . ? C26 C27 1.541(4) . ? 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 N1 P1 C12 111.92(13) . . ? N1 P1 C11 112.75(13) . . ? C12 P1 C11 105.65(13) . . ? N1 P1 C7 111.05(13) . . ? C12 P1 C7 102.38(13) . . ? C11 P1 C7 112.51(14) . . ? N2 P2 C19 114.14(12) . . ? N2 P2 C20 110.82(13) . . ? C19 P2 C20 103.73(13) . . ? N2 P2 C27 110.53(12) . . ? C19 P2 C27 104.50(13) . . ? C20 P2 C27 112.88(13) . . ? N1 Si1 C1 110.42(16) . . ? N1 Si1 C2 113.27(15) . . ? C1 Si1 C2 106.87(19) . . ? N1 Si1 C3 112.04(16) . . ? C1 Si1 C3 106.7(2) . . ? C2 Si1 C3 107.2(2) . . ? N2 Si2 C29 111.11(14) . . ? N2 Si2 C30 112.54(15) . . ? C29 Si2 C30 108.1(2) . . ? N2 Si2 C28 111.22(14) . . ? C29 Si2 C28 106.7(2) . . ? C30 Si2 C28 106.8(2) . . ? P1 N1 Si1 165.05(16) . . ? P2 N2 Si2 175.12(17) . . ? C5 C7 C6 107.3(3) . . ? C5 C7 C4 108.5(3) . . ? C6 C7 C4 109.8(3) . . ? C5 C7 P1 109.9(2) . . ? C6 C7 P1 106.8(2) . . ? C4 C7 P1 114.4(2) . . ? C10 C11 C8 109.8(2) . . ? C10 C11 C9 108.1(2) . . ? C8 C11 C9 107.6(2) . . ? C10 C11 P1 114.1(2) . . ? C8 C11 P1 111.3(2) . . ? C9 C11 P1 105.62(19) . . ? C13 C12 P1 117.80(18) . . ? C14 C13 C18 118.1(2) . . ? C14 C13 C12 120.0(2) . . ? C18 C13 C12 121.8(2) . . ? C15 C14 C13 120.4(2) . . ? C16 C15 C14 120.5(3) . . ? C15 C16 C17 120.6(2) . . ? C16 C17 C18 118.1(2) . . ? C16 C17 C19 120.2(2) . . ? C18 C17 C19 121.6(2) . . ? C13 C18 C17 122.2(2) . . ? C17 C19 P2 114.97(17) . . ? C23 C20 C22 108.1(2) . . ? C23 C20 C21 109.6(3) . . ? C22 C20 C21 108.0(3) . . ? C23 C20 P2 115.14(19) . . ? C22 C20 P2 106.0(2) . . ? C21 C20 P2 109.7(2) . . ? C24 C27 C26 109.9(3) . . ? C24 C27 C25 107.0(3) . . ? C26 C27 C25 108.4(3) . . ? C24 C27 P2 106.86(19) . . ? C26 C27 P2 114.9(2) . . ? C25 C27 P2 109.40(19) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 23.66 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.407 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.046 #===end data_m-C6H4(CH2(Cy2)PNSiMe3)2 _database_code_CSD 215281 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C38 H70 N2 P2 Si2' _chemical_formula_weight 673.08 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.541(6) _cell_length_b 15.118(8) _cell_length_c 15.328(9) _cell_angle_alpha 67.282(9) _cell_angle_beta 71.043(9) _cell_angle_gamma 75.162(10) _cell_volume 2107(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.274484 _exptl_absorpt_correction_T_max 0.488979 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8928 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 23.37 _reflns_number_total 6025 _reflns_number_gt 4583 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0909P)^2^+0.1695P] 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_number_reflns 6025 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 P1 P 0.95984(6) 0.21691(4) 0.30098(4) 0.03872(19) Uani 1 1 d . . . P2 P 0.57475(7) 0.28580(4) 0.70613(5) 0.0445(2) Uani 1 1 d . . . Si1 Si 0.65306(7) 0.29578(5) 0.29602(5) 0.0414(2) Uani 1 1 d . . . Si2 Si 0.53861(8) 0.09574(5) 0.68196(6) 0.0560(2) Uani 1 1 d . . . N1 N 0.8104(2) 0.26250(15) 0.30978(15) 0.0492(5) Uani 1 1 d . . . N2 N 0.5800(2) 0.19439(14) 0.68351(16) 0.0543(6) Uani 1 1 d . . . C1 C 1.0125(3) 0.11524(17) 0.25276(17) 0.0456(6) Uani 1 1 d . . . H1A H 1.1100 0.0944 0.2469 0.055 Uiso 1 1 calc R . . C2 C 0.9403(3) 0.02865(18) 0.3217(2) 0.0570(7) Uani 1 1 d . . . H2A H 0.8430 0.0496 0.3346 0.068 Uiso 1 1 calc R . . H2B H 0.9650 0.0048 0.3833 0.068 Uiso 1 1 calc R . . C3 C 0.9762(3) -0.0536(2) 0.2793(2) 0.0726(9) Uani 1 1 d . . . H3A H 1.0717 -0.0796 0.2732 0.087 Uiso 1 1 calc R . . H3B H 0.9242 -0.1053 0.3236 0.087 Uiso 1 1 calc R . . C4 C 0.9466(4) -0.0183(2) 0.1802(3) 0.0809(10) Uani 1 1 d . . . H4A H 0.9726 -0.0714 0.1542 0.097 Uiso 1 1 calc R . . H4B H 0.8500 0.0032 0.1871 0.097 Uiso 1 1 calc R . . C5 C 1.0230(4) 0.0642(2) 0.1101(2) 0.0786(10) Uani 1 1 d . . . H5A H 0.9999 0.0871 0.0480 0.094 Uiso 1 1 calc R . . H5B H 1.1198 0.0411 0.0989 0.094 Uiso 1 1 calc R . . C6 C 0.9893(3) 0.1481(2) 0.1500(2) 0.0636(8) Uani 1 1 d . . . H6A H 0.8952 0.1768 0.1526 0.076 Uiso 1 1 calc R . . H6B H 1.0454 0.1975 0.1058 0.076 Uiso 1 1 calc R . . C7 C 1.0792(2) 0.30456(17) 0.22794(17) 0.0453(6) Uani 1 1 d . . . H7A H 1.0733 0.3406 0.2706 0.054 Uiso 1 1 calc R . . C8 C 1.0396(3) 0.38145(19) 0.1381(2) 0.0575(7) Uani 1 1 d . . . H8A H 0.9479 0.4135 0.1574 0.069 Uiso 1 1 calc R . . H8B H 1.0409 0.3507 0.0928 0.069 Uiso 1 1 calc R . . C9 C 1.1357(3) 0.4566(2) 0.0874(2) 0.0683(8) Uani 1 1 d . . . H9A H 1.1122 0.5012 0.0276 0.082 Uiso 1 1 calc R . . H9B H 1.1247 0.4937 0.1295 0.082 Uiso 1 1 calc R . . C10 C 1.2831(3) 0.4100(2) 0.0632(2) 0.0723(9) Uani 1 1 d . . . H10A H 1.2967 0.3790 0.0154 0.087 Uiso 1 1 calc R . . H10B H 1.3414 0.4597 0.0347 0.087 Uiso 1 1 calc R . . C11 C 1.3213(3) 0.3360(2) 0.1536(2) 0.0713(8) Uani 1 1 d . . . H11A H 1.3171 0.3685 0.1983 0.086 Uiso 1 1 calc R . . H11B H 1.4139 0.3048 0.1357 0.086 Uiso 1 1 calc R . . C12 C 1.2281(3) 0.25998(19) 0.2044(2) 0.0568(7) Uani 1 1 d . . . H12A H 1.2517 0.2166 0.2646 0.068 Uiso 1 1 calc R . . H12B H 1.2413 0.2219 0.1629 0.068 Uiso 1 1 calc R . . C13 C 0.5410(3) 0.3510(2) 0.3902(2) 0.0664(8) Uani 1 1 d . . . H13A H 0.5776 0.4052 0.3854 0.100 Uiso 1 1 calc R . . H13B H 0.5360 0.3035 0.4541 0.100 Uiso 1 1 calc R . . H13C H 0.4517 0.3727 0.3793 0.100 Uiso 1 1 calc R . . C14 C 0.5747(3) 0.1912(2) 0.3101(2) 0.0679(8) Uani 1 1 d . . . H14A H 0.6292 0.1609 0.2627 0.102 Uiso 1 1 calc R . . H14B H 0.4850 0.2144 0.3003 0.102 Uiso 1 1 calc R . . H14C H 0.5698 0.1450 0.3747 0.102 Uiso 1 1 calc R . . C15 C 0.6487(3) 0.3897(2) 0.1737(2) 0.0664(8) Uani 1 1 d . . . H15A H 0.6882 0.4437 0.1659 0.100 Uiso 1 1 calc R . . H15B H 0.5564 0.4112 0.1693 0.100 Uiso 1 1 calc R . . H15C H 0.6993 0.3622 0.1233 0.100 Uiso 1 1 calc R . . C16 C 1.0031(3) 0.16488(18) 0.41954(17) 0.0464(6) Uani 1 1 d . . . H16A H 0.9509 0.1126 0.4613 0.056 Uiso 1 1 calc R . . H16B H 1.0984 0.1371 0.4093 0.056 Uiso 1 1 calc R . . C17 C 0.9770(2) 0.23706(18) 0.47188(16) 0.0445(6) Uani 1 1 d . . . C18 C 1.0823(3) 0.2696(2) 0.4807(2) 0.0624(8) Uani 1 1 d . . . H18A H 1.1717 0.2471 0.4539 0.075 Uiso 1 1 calc R . . C19 C 1.0553(3) 0.3354(3) 0.5290(2) 0.0751(9) Uani 1 1 d . . . H19A H 1.1268 0.3571 0.5341 0.090 Uiso 1 1 calc R . . C20 C 0.9246(3) 0.3690(2) 0.5695(2) 0.0631(8) Uani 1 1 d . . . H20A H 0.9081 0.4128 0.6025 0.076 Uiso 1 1 calc R . . C21 C 0.8153(3) 0.33822(17) 0.56183(17) 0.0469(6) Uani 1 1 d . . . C22 C 0.8447(3) 0.27172(17) 0.51244(16) 0.0437(6) Uani 1 1 d . . . H22A H 0.7737 0.2502 0.5067 0.052 Uiso 1 1 calc R . . C23 C 0.6703(3) 0.37539(17) 0.60224(18) 0.0512(7) Uani 1 1 d . . . H23A H 0.6241 0.4005 0.5502 0.061 Uiso 1 1 calc R . . H23B H 0.6685 0.4291 0.6225 0.061 Uiso 1 1 calc R . . C24 C 0.6556(3) 0.26352(19) 0.80406(19) 0.0559(7) Uani 1 1 d . . . H24A H 0.7527 0.2600 0.7715 0.067 Uiso 1 1 calc R . . C25 C 0.6437(4) 0.1658(2) 0.8835(2) 0.0756(9) Uani 1 1 d . . . H25A H 0.6747 0.1152 0.8539 0.091 Uiso 1 1 calc R . . H25B H 0.5492 0.1627 0.9187 0.091 Uiso 1 1 calc R . . C26 C 0.7269(4) 0.1483(3) 0.9547(2) 0.0832(10) Uani 1 1 d . . . H26A H 0.7112 0.0875 1.0072 0.100 Uiso 1 1 calc R . . H26B H 0.8225 0.1425 0.9210 0.100 Uiso 1 1 calc R . . C27 C 0.6927(5) 0.2281(3) 0.9973(3) 0.1057(14) Uani 1 1 d . . . H27A H 0.6009 0.2279 1.0388 0.127 Uiso 1 1 calc R . . H27B H 0.7536 0.2162 1.0377 0.127 Uiso 1 1 calc R . . C28 C 0.7038(5) 0.3251(3) 0.9201(3) 0.0999(13) Uani 1 1 d . . . H28A H 0.7987 0.3290 0.8869 0.120 Uiso 1 1 calc R . . H28B H 0.6705 0.3746 0.9511 0.120 Uiso 1 1 calc R . . C29 C 0.6259(4) 0.3469(2) 0.8445(2) 0.0700(9) Uani 1 1 d . . . H29A H 0.6503 0.4055 0.7911 0.084 Uiso 1 1 calc R . . H29B H 0.5294 0.3584 0.8741 0.084 Uiso 1 1 calc R . . C30 C 0.4029(3) 0.35265(18) 0.73533(18) 0.0517(7) Uani 1 1 d . . . H30A H 0.4099 0.4076 0.7516 0.062 Uiso 1 1 calc R . . C31 C 0.3104(3) 0.2889(2) 0.8241(2) 0.0677(8) Uani 1 1 d . . . H31A H 0.3460 0.2701 0.8807 0.081 Uiso 1 1 calc R . . H31B H 0.3105 0.2303 0.8123 0.081 Uiso 1 1 calc R . . C32 C 0.1642(3) 0.3407(3) 0.8462(2) 0.0814(10) Uani 1 1 d . . . H32A H 0.1080 0.2958 0.8994 0.098 Uiso 1 1 calc R . . H32B H 0.1621 0.3942 0.8670 0.098 Uiso 1 1 calc R . . C33 C 0.1067(3) 0.3791(3) 0.7572(2) 0.0796(10) Uani 1 1 d . . . H33A H 0.0996 0.3252 0.7404 0.096 Uiso 1 1 calc R . . H33B H 0.0163 0.4148 0.7723 0.096 Uiso 1 1 calc R . . C34 C 0.1960(3) 0.4444(2) 0.6720(2) 0.0724(9) Uani 1 1 d . . . H34A H 0.1966 0.5009 0.6872 0.087 Uiso 1 1 calc R . . H34B H 0.1590 0.4666 0.6155 0.087 Uiso 1 1 calc R . . C35 C 0.3410(3) 0.3933(2) 0.6469(2) 0.0584(7) Uani 1 1 d . . . H35A H 0.3961 0.4388 0.5935 0.070 Uiso 1 1 calc R . . H35B H 0.3416 0.3407 0.6254 0.070 Uiso 1 1 calc R . . C36 C 0.5111(5) -0.0002(3) 0.8053(3) 0.1177(16) Uani 1 1 d . . . H36A H 0.4404 0.0254 0.8512 0.177 Uiso 1 1 calc R . . H36B H 0.5934 -0.0203 0.8263 0.177 Uiso 1 1 calc R . . H36C H 0.4852 -0.0548 0.8015 0.177 Uiso 1 1 calc R . . C37 C 0.3826(4) 0.1226(3) 0.6379(3) 0.0970(12) Uani 1 1 d . . . H37A H 0.3942 0.1721 0.5748 0.146 Uiso 1 1 calc R . . H37B H 0.3060 0.1447 0.6832 0.146 Uiso 1 1 calc R . . H37C H 0.3675 0.0649 0.6332 0.146 Uiso 1 1 calc R . . C38 C 0.6776(3) 0.0424(2) 0.5964(2) 0.0746(9) Uani 1 1 d . . . H38A H 0.6937 0.0898 0.5322 0.112 Uiso 1 1 calc R . . H38B H 0.6518 -0.0131 0.5943 0.112 Uiso 1 1 calc R . . H38C H 0.7589 0.0229 0.6188 0.112 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 P1 0.0394(4) 0.0410(3) 0.0347(4) -0.0141(3) -0.0100(3) -0.0011(3) P2 0.0559(4) 0.0386(3) 0.0385(4) -0.0174(3) -0.0072(3) -0.0054(3) Si1 0.0401(4) 0.0413(4) 0.0445(4) -0.0148(3) -0.0137(3) -0.0038(3) Si2 0.0611(5) 0.0419(4) 0.0646(5) -0.0231(4) -0.0053(4) -0.0123(3) N1 0.0440(12) 0.0570(13) 0.0487(13) -0.0225(10) -0.0124(10) -0.0022(10) N2 0.0675(15) 0.0440(12) 0.0574(14) -0.0276(11) -0.0070(11) -0.0127(10) C1 0.0474(15) 0.0444(13) 0.0438(14) -0.0178(11) -0.0105(11) -0.0009(11) C2 0.0633(18) 0.0491(15) 0.0582(17) -0.0181(13) -0.0145(14) -0.0081(13) C3 0.079(2) 0.0480(16) 0.093(2) -0.0283(16) -0.0166(18) -0.0104(15) C4 0.086(2) 0.078(2) 0.099(3) -0.055(2) -0.018(2) -0.0128(18) C5 0.101(3) 0.079(2) 0.066(2) -0.0451(18) -0.0148(18) -0.0071(19) C6 0.086(2) 0.0624(17) 0.0501(17) -0.0306(14) -0.0178(15) -0.0047(15) C7 0.0446(15) 0.0444(13) 0.0448(15) -0.0142(11) -0.0110(11) -0.0046(11) C8 0.0542(17) 0.0513(15) 0.0581(18) -0.0066(13) -0.0185(14) -0.0056(13) C9 0.067(2) 0.0510(16) 0.070(2) -0.0024(14) -0.0142(16) -0.0125(14) C10 0.0588(19) 0.0701(19) 0.069(2) -0.0060(16) -0.0052(15) -0.0189(15) C11 0.0471(17) 0.079(2) 0.077(2) -0.0176(17) -0.0092(15) -0.0122(15) C12 0.0451(15) 0.0559(16) 0.0581(17) -0.0095(13) -0.0139(13) -0.0026(12) C13 0.0499(17) 0.0728(19) 0.078(2) -0.0392(17) -0.0084(15) 0.0003(14) C14 0.071(2) 0.0564(17) 0.086(2) -0.0199(16) -0.0312(17) -0.0163(15) C15 0.076(2) 0.0602(17) 0.0623(19) -0.0036(14) -0.0342(16) -0.0133(15) C16 0.0461(14) 0.0506(14) 0.0378(14) -0.0146(11) -0.0106(11) 0.0005(11) C17 0.0467(15) 0.0534(14) 0.0327(13) -0.0128(11) -0.0119(11) -0.0062(12) C18 0.0484(17) 0.092(2) 0.0535(17) -0.0296(16) -0.0136(13) -0.0114(15) C19 0.071(2) 0.107(3) 0.069(2) -0.040(2) -0.0152(17) -0.0362(19) C20 0.080(2) 0.0708(18) 0.0534(17) -0.0295(15) -0.0139(15) -0.0265(16) C21 0.0609(17) 0.0460(14) 0.0328(13) -0.0120(11) -0.0082(12) -0.0125(12) C22 0.0517(15) 0.0466(13) 0.0352(13) -0.0125(11) -0.0111(11) -0.0131(11) C23 0.0709(18) 0.0406(13) 0.0404(14) -0.0153(11) -0.0090(12) -0.0090(12) C24 0.0687(19) 0.0566(16) 0.0453(16) -0.0197(13) -0.0130(13) -0.0114(13) C25 0.099(3) 0.0606(18) 0.063(2) -0.0182(16) -0.0280(18) 0.0011(17) C26 0.097(3) 0.085(2) 0.058(2) -0.0230(18) -0.0309(18) 0.015(2) C27 0.133(3) 0.124(3) 0.077(3) -0.052(3) -0.055(2) 0.019(3) C28 0.140(4) 0.104(3) 0.089(3) -0.047(2) -0.047(3) -0.024(3) C29 0.096(2) 0.0636(18) 0.0642(19) -0.0337(16) -0.0277(17) -0.0054(16) C30 0.0619(17) 0.0489(14) 0.0454(15) -0.0240(12) -0.0104(13) -0.0012(12) C31 0.0647(19) 0.0765(19) 0.0545(18) -0.0252(16) -0.0061(14) -0.0044(15) C32 0.067(2) 0.104(3) 0.064(2) -0.0356(19) -0.0012(16) -0.0056(19) C33 0.061(2) 0.100(3) 0.082(2) -0.043(2) -0.0163(17) 0.0002(18) C34 0.075(2) 0.074(2) 0.077(2) -0.0364(18) -0.0310(18) 0.0080(17) C35 0.0676(19) 0.0555(16) 0.0525(17) -0.0229(13) -0.0149(14) -0.0022(14) C36 0.191(5) 0.067(2) 0.083(3) -0.009(2) -0.008(3) -0.057(3) C37 0.067(2) 0.085(2) 0.157(4) -0.058(3) -0.026(2) -0.0170(18) C38 0.073(2) 0.0618(18) 0.099(2) -0.0477(18) -0.0128(18) -0.0049(15) _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 P1 N1 1.533(2) . ? P1 C16 1.839(2) . ? P1 C7 1.840(3) . ? P1 C1 1.841(2) . ? P2 N2 1.533(2) . ? P2 C23 1.837(3) . ? P2 C24 1.841(3) . ? P2 C30 1.841(3) . ? Si1 N1 1.664(2) . ? Si1 C13 1.869(3) . ? Si1 C15 1.870(3) . ? Si1 C14 1.875(3) . ? Si2 N2 1.668(2) . ? Si2 C38 1.865(3) . ? Si2 C37 1.869(4) . ? Si2 C36 1.871(4) . ? C1 C2 1.526(4) . ? C1 C6 1.539(4) . ? C2 C3 1.527(4) . ? C3 C4 1.512(5) . ? C4 C5 1.509(5) . ? C5 C6 1.528(4) . ? C7 C8 1.520(3) . ? C7 C12 1.525(3) . ? C8 C9 1.523(4) . ? C9 C10 1.522(4) . ? C10 C11 1.506(4) . ? C11 C12 1.510(4) . ? C16 C17 1.513(3) . ? C17 C18 1.386(4) . ? C17 C22 1.386(3) . ? C18 C19 1.380(4) . ? C19 C20 1.368(4) . ? C20 C21 1.401(4) . ? C21 C22 1.398(3) . ? C21 C23 1.500(4) . ? C24 C25 1.512(4) . ? C24 C29 1.531(4) . ? C25 C26 1.520(4) . ? C26 C27 1.499(5) . ? C27 C28 1.491(5) . ? C28 C29 1.520(5) . ? C30 C31 1.529(4) . ? C30 C35 1.538(4) . ? C31 C32 1.532(4) . ? C32 C33 1.521(5) . ? C33 C34 1.499(5) . ? C34 C35 1.525(4) . ? 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 N1 P1 C16 112.63(11) . . ? N1 P1 C7 113.67(12) . . ? C16 P1 C7 102.88(12) . . ? N1 P1 C1 114.91(12) . . ? C16 P1 C1 103.82(11) . . ? C7 P1 C1 107.80(12) . . ? N2 P2 C23 112.42(12) . . ? N2 P2 C24 113.80(12) . . ? C23 P2 C24 102.58(13) . . ? N2 P2 C30 114.24(13) . . ? C23 P2 C30 104.38(12) . . ? C24 P2 C30 108.38(12) . . ? N1 Si1 C13 110.41(12) . . ? N1 Si1 C15 110.92(12) . . ? C13 Si1 C15 106.97(14) . . ? N1 Si1 C14 112.74(12) . . ? C13 Si1 C14 106.77(15) . . ? C15 Si1 C14 108.79(14) . . ? N2 Si2 C38 109.98(13) . . ? N2 Si2 C37 112.72(14) . . ? C38 Si2 C37 106.26(17) . . ? N2 Si2 C36 112.14(15) . . ? C38 Si2 C36 107.49(18) . . ? C37 Si2 C36 108.0(2) . . ? P1 N1 Si1 163.07(15) . . ? P2 N2 Si2 162.49(16) . . ? C2 C1 C6 110.9(2) . . ? C2 C1 P1 111.78(17) . . ? C6 C1 P1 110.64(17) . . ? C1 C2 C3 112.2(2) . . ? C4 C3 C2 111.1(2) . . ? C5 C4 C3 110.9(3) . . ? C4 C5 C6 111.3(3) . . ? C5 C6 C1 112.3(2) . . ? C8 C7 C12 111.8(2) . . ? C8 C7 P1 114.75(18) . . ? C12 C7 P1 115.08(17) . . ? C7 C8 C9 111.5(2) . . ? C10 C9 C8 111.9(2) . . ? C11 C10 C9 110.8(2) . . ? C10 C11 C12 111.7(3) . . ? C11 C12 C7 112.2(2) . . ? C17 C16 P1 114.10(16) . . ? C18 C17 C22 118.7(2) . . ? C18 C17 C16 121.7(2) . . ? C22 C17 C16 119.5(2) . . ? C19 C18 C17 120.4(3) . . ? C20 C19 C18 120.7(3) . . ? C19 C20 C21 120.7(3) . . ? C22 C21 C20 117.8(2) . . ? C22 C21 C23 119.6(2) . . ? C20 C21 C23 122.6(2) . . ? C17 C22 C21 121.7(2) . . ? C21 C23 P2 115.31(17) . . ? C25 C24 C29 112.9(2) . . ? C25 C24 P2 114.8(2) . . ? C29 C24 P2 115.41(19) . . ? C24 C25 C26 111.5(3) . . ? C27 C26 C25 112.5(3) . . ? C28 C27 C26 112.0(3) . . ? C27 C28 C29 114.1(3) . . ? C28 C29 C24 111.9(3) . . ? C31 C30 C35 110.5(2) . . ? C31 C30 P2 111.22(18) . . ? C35 C30 P2 111.17(17) . . ? C30 C31 C32 112.4(3) . . ? C33 C32 C31 111.6(3) . . ? C34 C33 C32 110.5(3) . . ? C33 C34 C35 112.0(3) . . ? C34 C35 C30 111.5(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.381 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.047 #===end data_m-C6H4(CH2(t-Bu2)PNH)2 _database_code_CSD 215282 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H46 N2 P2' _chemical_formula_weight 424.57 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.457(8) _cell_length_b 13.908(8) _cell_length_c 14.713(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.388(10) _cell_angle_gamma 90.00 _cell_volume 2613(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.321773 _exptl_absorpt_correction_T_max 0.488950 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 10896 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.17 _reflns_number_total 3714 _reflns_number_gt 2709 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0897P)^2^+0.0000P] 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_number_reflns 3714 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _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 P1 P 0.70529(5) 0.81918(5) -0.22319(5) 0.0429(2) Uani 1 1 d . . . P2 P 0.77437(5) 0.97172(4) 0.20935(4) 0.0393(2) Uani 1 1 d . . . N1 N 0.7683(2) 0.91622(18) -0.19604(17) 0.0644(7) Uani 1 1 d . . . N2 N 0.80992(19) 0.86285(16) 0.22209(16) 0.0605(7) Uani 1 1 d . . . C1 C 0.57446(19) 0.8256(2) -0.20723(18) 0.0481(7) Uani 1 1 d . . . H1A H 0.5389 0.8815 -0.2420 0.058 Uiso 1 1 calc R . . H1B H 0.5352 0.7695 -0.2380 0.058 Uiso 1 1 calc R . . C2 C 0.56699(18) 0.83095(18) -0.10718(18) 0.0415(6) Uani 1 1 d . . . C3 C 0.5100(2) 0.76182(19) -0.0759(2) 0.0499(7) Uani 1 1 d . . . H3A H 0.4779 0.7116 -0.1162 0.060 Uiso 1 1 calc R . . C4 C 0.5011(2) 0.7679(2) 0.0150(2) 0.0575(8) Uani 1 1 d . . . H4A H 0.4627 0.7218 0.0353 0.069 Uiso 1 1 calc R . . C5 C 0.5485(2) 0.8416(2) 0.0760(2) 0.0543(7) Uani 1 1 d . . . H5A H 0.5434 0.8436 0.1376 0.065 Uiso 1 1 calc R . . C6 C 0.60415(18) 0.91359(17) 0.04639(18) 0.0423(6) Uani 1 1 d . . . C7 C 0.61193(19) 0.90639(18) -0.04570(18) 0.0430(6) Uani 1 1 d . . . H7A H 0.6484 0.9536 -0.0668 0.052 Uiso 1 1 calc R . . C8 C 0.6706(2) 0.7986(2) -0.35538(19) 0.0617(8) Uani 1 1 d . . . C9 C 0.7692(3) 0.8100(3) -0.3862(2) 0.0920(12) Uani 1 1 d . . . H9A H 0.7513 0.7999 -0.4540 0.138 Uiso 1 1 calc R . . H9B H 0.8208 0.7637 -0.3530 0.138 Uiso 1 1 calc R . . H9C H 0.7970 0.8737 -0.3707 0.138 Uiso 1 1 calc R . . C10 C 0.5924(3) 0.8798(3) -0.4060(2) 0.0871(12) Uani 1 1 d . . . H10A H 0.5731 0.8717 -0.4742 0.131 Uiso 1 1 calc R . . H10B H 0.6252 0.9413 -0.3886 0.131 Uiso 1 1 calc R . . H10C H 0.5309 0.8762 -0.3864 0.131 Uiso 1 1 calc R . . C11 C 0.6202(3) 0.7004(3) -0.3883(2) 0.0882(11) Uani 1 1 d . . . H11A H 0.6046 0.6947 -0.4564 0.132 Uiso 1 1 calc R . . H11B H 0.5568 0.6948 -0.3720 0.132 Uiso 1 1 calc R . . H11C H 0.6679 0.6503 -0.3570 0.132 Uiso 1 1 calc R . . C12 C 0.7747(2) 0.7140(2) -0.1517(2) 0.0563(7) Uani 1 1 d . . . C13 C 0.8208(3) 0.7494(2) -0.0477(2) 0.0760(10) Uani 1 1 d . . . H13A H 0.8575 0.6976 -0.0080 0.114 Uiso 1 1 calc R . . H13B H 0.7652 0.7712 -0.0250 0.114 Uiso 1 1 calc R . . H13C H 0.8686 0.8014 -0.0452 0.114 Uiso 1 1 calc R . . C14 C 0.7036(3) 0.6272(2) -0.1530(3) 0.0780(10) Uani 1 1 d . . . H14A H 0.7444 0.5762 -0.1152 0.117 Uiso 1 1 calc R . . H14B H 0.6726 0.6055 -0.2177 0.117 Uiso 1 1 calc R . . H14C H 0.6494 0.6457 -0.1269 0.117 Uiso 1 1 calc R . . C15 C 0.8678(3) 0.6821(3) -0.1856(3) 0.0808(10) Uani 1 1 d . . . H15A H 0.9023 0.6280 -0.1483 0.121 Uiso 1 1 calc R . . H15B H 0.9166 0.7343 -0.1776 0.121 Uiso 1 1 calc R . . H15C H 0.8421 0.6643 -0.2520 0.121 Uiso 1 1 calc R . . C16 C 0.6513(2) 0.99825(18) 0.11034(18) 0.0475(7) Uani 1 1 d . . . H16A H 0.5998 1.0226 0.1381 0.057 Uiso 1 1 calc R . . H16B H 0.6656 1.0490 0.0709 0.057 Uiso 1 1 calc R . . C17 C 0.8739(2) 1.0512(2) 0.18136(19) 0.0528(7) Uani 1 1 d . . . C18 C 0.8423(3) 1.1568(2) 0.1597(3) 0.0821(11) Uani 1 1 d . . . H18A H 0.8977 1.1908 0.1456 0.123 Uiso 1 1 calc R . . H18B H 0.8295 1.1854 0.2143 0.123 Uiso 1 1 calc R . . H18C H 0.7798 1.1602 0.1055 0.123 Uiso 1 1 calc R . . C19 C 0.8915(3) 1.0060(3) 0.0925(2) 0.0819(11) Uani 1 1 d . . . H19A H 0.9416 1.0436 0.0737 0.123 Uiso 1 1 calc R . . H19B H 0.8265 1.0044 0.0410 0.123 Uiso 1 1 calc R . . H19C H 0.9176 0.9417 0.1071 0.123 Uiso 1 1 calc R . . C20 C 0.9775(3) 1.0455(3) 0.2631(3) 0.1015(13) Uani 1 1 d . . . H20A H 1.0284 1.0860 0.2488 0.152 Uiso 1 1 calc R . . H20B H 1.0022 0.9803 0.2703 0.152 Uiso 1 1 calc R . . H20C H 0.9670 1.0667 0.3215 0.152 Uiso 1 1 calc R . . C21 C 0.7472(2) 1.00963(19) 0.32105(19) 0.0513(7) Uani 1 1 d . . . C22 C 0.6514(3) 0.9523(2) 0.3264(3) 0.0849(11) Uani 1 1 d . . . H22A H 0.6352 0.9702 0.3831 0.127 Uiso 1 1 calc R . . H22B H 0.6667 0.8847 0.3284 0.127 Uiso 1 1 calc R . . H22C H 0.5925 0.9661 0.2710 0.127 Uiso 1 1 calc R . . C23 C 0.7227(3) 1.1174(2) 0.3233(2) 0.0660(9) Uani 1 1 d . . . H23A H 0.7097 1.1324 0.3822 0.099 Uiso 1 1 calc R . . H23B H 0.6619 1.1328 0.2703 0.099 Uiso 1 1 calc R . . H23C H 0.7813 1.1542 0.3189 0.099 Uiso 1 1 calc R . . C24 C 0.8398(3) 0.9833(3) 0.4103(2) 0.0934(12) Uani 1 1 d . . . H24A H 0.8247 1.0035 0.4669 0.140 Uiso 1 1 calc R . . H24B H 0.9020 1.0151 0.4072 0.140 Uiso 1 1 calc R . . H24C H 0.8505 0.9150 0.4123 0.140 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 P1 0.0430(4) 0.0503(5) 0.0341(4) -0.0014(3) 0.0102(3) -0.0082(3) P2 0.0449(4) 0.0340(4) 0.0362(4) -0.0011(3) 0.0089(3) 0.0039(3) N1 0.0711(17) 0.0617(16) 0.0557(16) -0.0001(12) 0.0131(12) -0.0242(13) N2 0.0691(16) 0.0392(14) 0.0625(16) 0.0043(11) 0.0055(12) 0.0142(11) C1 0.0429(15) 0.0553(17) 0.0428(16) -0.0044(12) 0.0087(12) -0.0038(12) C2 0.0344(13) 0.0475(15) 0.0406(15) -0.0051(12) 0.0091(11) 0.0008(12) C3 0.0457(16) 0.0502(17) 0.0546(18) -0.0125(13) 0.0169(13) -0.0096(13) C4 0.0580(18) 0.0593(18) 0.0606(19) -0.0065(15) 0.0262(15) -0.0186(15) C5 0.0582(18) 0.0644(19) 0.0428(16) -0.0054(14) 0.0197(13) -0.0060(15) C6 0.0360(14) 0.0442(15) 0.0439(16) -0.0033(12) 0.0085(11) 0.0027(11) C7 0.0357(14) 0.0439(15) 0.0473(16) 0.0011(12) 0.0100(11) -0.0026(11) C8 0.0607(19) 0.089(2) 0.0369(16) -0.0095(15) 0.0168(14) -0.0213(17) C9 0.082(2) 0.153(4) 0.052(2) -0.006(2) 0.0358(18) -0.024(2) C10 0.085(2) 0.121(3) 0.0435(19) 0.0154(19) 0.0030(16) -0.014(2) C11 0.093(3) 0.114(3) 0.060(2) -0.042(2) 0.0274(18) -0.036(2) C12 0.0556(17) 0.0577(18) 0.0589(19) 0.0053(14) 0.0226(14) 0.0076(14) C13 0.073(2) 0.095(3) 0.052(2) 0.0173(17) 0.0079(16) 0.0211(19) C14 0.091(3) 0.0517(19) 0.107(3) 0.0148(18) 0.055(2) 0.0094(18) C15 0.067(2) 0.093(3) 0.092(3) 0.011(2) 0.0388(19) 0.0188(19) C16 0.0480(16) 0.0424(15) 0.0463(16) -0.0037(12) 0.0067(12) 0.0048(12) C17 0.0516(17) 0.0562(18) 0.0525(17) -0.0061(13) 0.0191(14) -0.0069(13) C18 0.106(3) 0.054(2) 0.099(3) 0.0042(18) 0.050(2) -0.0171(19) C19 0.089(3) 0.090(3) 0.085(3) -0.012(2) 0.054(2) -0.006(2) C20 0.056(2) 0.140(4) 0.098(3) 0.000(3) 0.010(2) -0.026(2) C21 0.0664(19) 0.0467(16) 0.0425(16) 0.0010(12) 0.0196(13) 0.0053(14) C22 0.121(3) 0.070(2) 0.087(3) 0.0021(19) 0.065(2) -0.007(2) C23 0.085(2) 0.0570(19) 0.064(2) -0.0172(15) 0.0348(17) 0.0034(16) C24 0.119(3) 0.115(3) 0.0402(19) 0.0100(19) 0.0157(19) 0.039(3) _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 P1 N1 1.577(2) . ? P1 C1 1.850(3) . ? P1 C12 1.870(3) . ? P1 C8 1.873(3) . ? P2 N2 1.581(2) . ? P2 C21 1.869(3) . ? P2 C17 1.879(3) . ? P2 C16 1.865(3) . ? C1 C2 1.509(4) . ? C2 C7 1.393(3) . ? C2 C3 1.396(4) . ? C3 C4 1.382(4) . ? C4 C5 1.380(4) . ? C5 C6 1.399(4) . ? C6 C7 1.395(3) . ? C6 C16 1.516(3) . ? C8 C11 1.533(4) . ? C8 C9 1.540(4) . ? C8 C10 1.563(5) . ? C12 C14 1.537(4) . ? C12 C15 1.552(4) . ? C12 C13 1.539(4) . ? C17 C19 1.536(4) . ? C17 C18 1.534(4) . ? C17 C20 1.530(4) . ? C21 C23 1.537(4) . ? C21 C24 1.543(4) . ? C21 C22 1.539(4) . ? 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 N1 P1 C1 112.60(13) . . ? N1 P1 C12 113.14(14) . . ? C1 P1 C12 107.02(13) . . ? N1 P1 C8 109.40(13) . . ? C1 P1 C8 101.74(12) . . ? C12 P1 C8 112.40(14) . . ? N2 P2 C21 107.57(13) . . ? N2 P2 C17 112.30(14) . . ? C21 P2 C17 112.17(13) . . ? N2 P2 C16 116.29(12) . . ? C21 P2 C16 105.02(13) . . ? C17 P2 C16 103.34(13) . . ? C2 C1 P1 119.02(17) . . ? C7 C2 C3 118.4(2) . . ? C7 C2 C1 121.5(2) . . ? C3 C2 C1 120.0(2) . . ? C4 C3 C2 120.1(2) . . ? C3 C4 C5 120.8(3) . . ? C6 C5 C4 120.8(3) . . ? C5 C6 C7 117.6(2) . . ? C5 C6 C16 121.5(2) . . ? C7 C6 C16 120.9(2) . . ? C2 C7 C6 122.3(2) . . ? C11 C8 C9 109.6(3) . . ? C11 C8 C10 109.2(3) . . ? C9 C8 C10 107.3(3) . . ? C11 C8 P1 113.9(2) . . ? C9 C8 P1 109.5(2) . . ? C10 C8 P1 107.1(2) . . ? C14 C12 C15 109.5(3) . . ? C14 C12 C13 108.5(3) . . ? C15 C12 C13 107.4(3) . . ? C14 C12 P1 114.1(2) . . ? C15 C12 P1 110.7(2) . . ? C13 C12 P1 106.4(2) . . ? C6 C16 P2 115.21(17) . . ? C19 C17 C18 108.8(3) . . ? C19 C17 C20 107.5(3) . . ? C18 C17 C20 109.7(3) . . ? C19 C17 P2 105.0(2) . . ? C18 C17 P2 116.0(2) . . ? C20 C17 P2 109.5(2) . . ? C23 C21 C24 109.5(3) . . ? C23 C21 C22 108.4(3) . . ? C24 C21 C22 107.4(3) . . ? C23 C21 P2 113.37(19) . . ? C24 C21 P2 110.6(2) . . ? C22 C21 P2 107.3(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.17 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.357 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.054 #===end data_m-C6H4(CH2(Cy2)PN)2Ti(NMe2)2 _database_code_CSD 215283 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_formula_sum 'C36 H64 N4 P2 Ti' _chemical_formula_weight 662.75 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' N N 0.0061 0.0033 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.726(5) _cell_length_b 12.389(8) _cell_length_c 18.381(11) _cell_angle_alpha 102.835(11) _cell_angle_beta 93.060(12) _cell_angle_gamma 90.686(12) _cell_volume 1934(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.167631 _exptl_absorpt_correction_T_max 0.256568 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8246 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 23.29 _reflns_number_total 5491 _reflns_number_gt 3079 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1593P)^2^+0.0000P] 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_number_reflns 5491 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.2154 _refine_ls_wR_factor_gt 0.1975 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 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 Ti1 Ti 0.86014(9) -0.00402(8) 0.27063(5) 0.0488(3) Uani 1 1 d . . . P1 P 0.74835(16) 0.25725(12) 0.31089(8) 0.0578(4) Uani 1 1 d . . . P2 P 0.71421(15) -0.15990(11) 0.10700(7) 0.0497(4) Uani 1 1 d . . . N1 N 0.8384(5) 0.1497(4) 0.2837(2) 0.0604(12) Uani 1 1 d . . . N2 N 0.8138(5) -0.0873(3) 0.1740(2) 0.0560(11) Uani 1 1 d . . . N3 N 0.7383(5) -0.0578(4) 0.3401(2) 0.0655(12) Uani 1 1 d . . . N4 N 1.0634(5) -0.0331(4) 0.3026(2) 0.0613(12) Uani 1 1 d . . . C1 C 0.5795(5) 0.1036(4) 0.1486(3) 0.0498(13) Uani 1 1 d . . . H1A H 0.6809 0.1123 0.1373 0.060 Uiso 1 1 calc R . . C2 C 0.5145(6) 0.1882(5) 0.2000(3) 0.0547(13) Uani 1 1 d . . . C3 C 0.3626(7) 0.1720(6) 0.2148(3) 0.0720(17) Uani 1 1 d . . . H3A H 0.3154 0.2266 0.2488 0.086 Uiso 1 1 calc R . . C4 C 0.2802(6) 0.0780(6) 0.1807(3) 0.0750(18) Uani 1 1 d . . . H4A H 0.1783 0.0703 0.1915 0.090 Uiso 1 1 calc R . . C5 C 0.3465(6) -0.0055(5) 0.1306(3) 0.0653(15) Uani 1 1 d . . . H5A H 0.2901 -0.0696 0.1085 0.078 Uiso 1 1 calc R . . C6 C 0.4986(6) 0.0065(4) 0.1133(3) 0.0514(13) Uani 1 1 d . . . C7 C 0.6115(6) 0.2877(5) 0.2381(3) 0.0659(15) Uani 1 1 d . . . H7A H 0.5452 0.3465 0.2608 0.079 Uiso 1 1 calc R . . H7B H 0.6682 0.3137 0.2011 0.079 Uiso 1 1 calc R . . C8 C 0.6284(7) 0.2520(5) 0.3898(3) 0.0662(15) Uani 1 1 d . . . H8A H 0.5580 0.1884 0.3716 0.079 Uiso 1 1 calc R . . C9 C 0.5257(8) 0.3502(6) 0.4156(3) 0.090(2) Uani 1 1 d . . . H9A H 0.4606 0.3618 0.3737 0.108 Uiso 1 1 calc R . . H9B H 0.5885 0.4167 0.4345 0.108 Uiso 1 1 calc R . . C10 C 0.4250(9) 0.3278(7) 0.4778(4) 0.115(3) Uani 1 1 d . . . H10A H 0.3609 0.3912 0.4938 0.138 Uiso 1 1 calc R . . H10B H 0.3576 0.2644 0.4570 0.138 Uiso 1 1 calc R . . C11 C 0.5116(10) 0.3070(7) 0.5428(4) 0.106(3) Uani 1 1 d . . . H11A H 0.4420 0.2915 0.5788 0.127 Uiso 1 1 calc R . . H11B H 0.5746 0.3716 0.5664 0.127 Uiso 1 1 calc R . . C12 C 0.6137(10) 0.2070(7) 0.5168(4) 0.110(3) Uani 1 1 d . . . H12A H 0.5491 0.1417 0.4971 0.132 Uiso 1 1 calc R . . H12B H 0.6754 0.1939 0.5593 0.132 Uiso 1 1 calc R . . C13 C 0.7211(8) 0.2251(6) 0.4559(3) 0.089(2) Uani 1 1 d . . . H13A H 0.7934 0.2855 0.4769 0.107 Uiso 1 1 calc R . . H13B H 0.7790 0.1588 0.4389 0.107 Uiso 1 1 calc R . . C14 C 0.8708(8) 0.3821(6) 0.3375(4) 0.089(2) Uiso 1 1 d . . . C15 C 0.8130(15) 0.4865(12) 0.3433(7) 0.086(4) Uiso 0.50 1 d P . . C15A C 0.9379(18) 0.4075(13) 0.2555(8) 0.105(5) Uiso 0.50 1 d P . . C16 C 0.9339(19) 0.5881(15) 0.3738(9) 0.114(5) Uiso 0.50 1 d P . . C16A C 1.024(2) 0.5360(17) 0.2733(11) 0.136(6) Uiso 0.50 1 d P . . C17 C 1.1034(14) 0.5558(10) 0.3312(6) 0.155(4) Uiso 1 1 d . . . C18 C 1.1565(17) 0.4642(13) 0.3287(8) 0.096(4) Uiso 0.50 1 d P . . C18A C 1.066(3) 0.518(2) 0.4038(13) 0.169(8) Uiso 0.50 1 d P . . C19 C 1.0287(16) 0.3577(11) 0.3011(7) 0.086(4) Uiso 0.50 1 d P . . C19A C 0.972(2) 0.3860(15) 0.3825(10) 0.122(5) Uiso 0.50 1 d P . . C20 C 0.5775(6) -0.0811(4) 0.0593(3) 0.0600(14) Uani 1 1 d . . . H20A H 0.6325 -0.0465 0.0256 0.072 Uiso 1 1 calc R . . H20B H 0.5009 -0.1320 0.0295 0.072 Uiso 1 1 calc R . . C21 C 0.8283(6) -0.2304(5) 0.0296(3) 0.0653(15) Uiso 1 1 d . . . C22 C 0.9271(10) -0.3176(7) 0.0497(5) 0.083(2) Uiso 0.75 1 d P . . C22A C 0.769(2) -0.2710(16) -0.0404(10) 0.049(5) Uiso 0.25 1 d P . . C23 C 1.0222(12) -0.3734(9) -0.0218(6) 0.106(3) Uiso 0.75 1 d P . . C23A C 0.889(3) -0.338(2) -0.0963(14) 0.084(7) Uiso 0.25 1 d P . . C24 C 1.1160(13) -0.2845(11) -0.0428(6) 0.103(3) Uiso 0.75 1 d P . . C24A C 1.021(3) -0.268(2) -0.0945(13) 0.066(6) Uiso 0.25 1 d P . . C25 C 1.0139(13) -0.1967(10) -0.0704(6) 0.103(3) Uiso 0.75 1 d P . . C25A C 1.109(4) -0.212(3) -0.0227(19) 0.109(10) Uiso 0.25 1 d P . . C26 C 0.9175(11) -0.1380(8) -0.0004(5) 0.085(3) Uiso 0.75 1 d P . . C26A C 0.979(3) -0.153(2) 0.0354(13) 0.067(6) Uiso 0.25 1 d P . . C27 C 0.5861(6) -0.2609(5) 0.1347(3) 0.0622(15) Uani 1 1 d . . . H27A H 0.5048 -0.2167 0.1606 0.075 Uiso 1 1 calc R . . C28 C 0.6621(7) -0.3174(6) 0.1928(4) 0.0831(19) Uani 1 1 d . . . H28A H 0.7097 -0.2621 0.2338 0.100 Uiso 1 1 calc R . . H28B H 0.7412 -0.3661 0.1703 0.100 Uiso 1 1 calc R . . C29 C 0.5371(10) -0.3861(7) 0.2228(4) 0.113(3) Uani 1 1 d . . . H29A H 0.5857 -0.4242 0.2583 0.136 Uiso 1 1 calc R . . H29B H 0.4631 -0.3360 0.2488 0.136 Uiso 1 1 calc R . . C30 C 0.4559(10) -0.4684(6) 0.1614(5) 0.116(3) Uani 1 1 d . . . H30A H 0.3767 -0.5068 0.1816 0.140 Uiso 1 1 calc R . . H30B H 0.5280 -0.5228 0.1383 0.140 Uiso 1 1 calc R . . C31 C 0.3846(8) -0.4134(6) 0.1035(4) 0.099(2) Uani 1 1 d . . . H31A H 0.3052 -0.3646 0.1256 0.119 Uiso 1 1 calc R . . H31B H 0.3365 -0.4694 0.0631 0.119 Uiso 1 1 calc R . . C32 C 0.5022(8) -0.3462(5) 0.0718(3) 0.0825(18) Uani 1 1 d . . . H32A H 0.5759 -0.3956 0.0449 0.099 Uiso 1 1 calc R . . H32B H 0.4503 -0.3086 0.0368 0.099 Uiso 1 1 calc R . . C33 C 0.7871(9) -0.1010(8) 0.4032(4) 0.118(3) Uani 1 1 d . . . H33A H 0.6989 -0.1215 0.4265 0.177 Uiso 1 1 calc R . . H33B H 0.8471 -0.0455 0.4383 0.177 Uiso 1 1 calc R . . H33C H 0.8482 -0.1649 0.3871 0.177 Uiso 1 1 calc R . . C34 C 0.5760(6) -0.0613(5) 0.3296(3) 0.0802(18) Uani 1 1 d . . . H34A H 0.5322 -0.0904 0.3683 0.120 Uiso 1 1 calc R . . H34B H 0.5459 -0.1079 0.2818 0.120 Uiso 1 1 calc R . . H34C H 0.5399 0.0122 0.3316 0.120 Uiso 1 1 calc R . . C35 C 1.1419(8) -0.1359(6) 0.2749(4) 0.095(2) Uani 1 1 d . . . H35A H 1.2430 -0.1318 0.2988 0.143 Uiso 1 1 calc R . . H35B H 1.1493 -0.1471 0.2218 0.143 Uiso 1 1 calc R . . H35C H 1.0850 -0.1967 0.2858 0.143 Uiso 1 1 calc R . . C36 C 1.1554(7) 0.0433(6) 0.3616(3) 0.092(2) Uani 1 1 d . . . H36A H 1.2539 0.0122 0.3685 0.138 Uiso 1 1 calc R . . H36B H 1.1037 0.0549 0.4074 0.138 Uiso 1 1 calc R . . H36C H 1.1688 0.1127 0.3474 0.138 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 Ti1 0.0394(5) 0.0563(7) 0.0486(6) 0.0082(4) -0.0009(4) -0.0021(4) P1 0.0560(8) 0.0517(9) 0.0625(9) 0.0046(7) 0.0094(7) -0.0030(7) P2 0.0505(8) 0.0548(9) 0.0431(7) 0.0103(6) -0.0016(6) -0.0006(6) N1 0.057(3) 0.061(3) 0.059(3) 0.005(2) -0.001(2) 0.000(2) N2 0.057(3) 0.056(3) 0.052(2) 0.008(2) -0.008(2) 0.007(2) N3 0.057(3) 0.077(3) 0.062(3) 0.014(2) 0.004(2) -0.002(2) N4 0.044(2) 0.071(3) 0.068(3) 0.016(2) -0.008(2) -0.001(2) C1 0.044(3) 0.062(4) 0.051(3) 0.028(3) 0.006(2) 0.005(3) C2 0.056(3) 0.059(4) 0.055(3) 0.023(3) 0.008(3) 0.011(3) C3 0.060(4) 0.089(5) 0.072(4) 0.023(3) 0.018(3) 0.023(4) C4 0.043(3) 0.108(6) 0.079(4) 0.030(4) 0.013(3) -0.001(4) C5 0.052(3) 0.081(4) 0.067(3) 0.028(3) -0.008(3) -0.012(3) C6 0.052(3) 0.060(4) 0.046(3) 0.022(3) -0.002(2) 0.005(3) C7 0.071(4) 0.058(4) 0.073(4) 0.021(3) 0.016(3) 0.018(3) C8 0.072(4) 0.061(4) 0.062(3) 0.003(3) 0.012(3) -0.005(3) C9 0.081(4) 0.103(6) 0.079(4) 0.002(4) 0.018(4) 0.015(4) C10 0.096(5) 0.119(7) 0.107(6) -0.029(5) 0.037(5) 0.004(5) C11 0.119(6) 0.111(7) 0.077(5) -0.007(4) 0.033(5) -0.025(5) C12 0.145(7) 0.111(7) 0.079(5) 0.031(4) 0.032(5) -0.001(5) C13 0.101(5) 0.097(5) 0.069(4) 0.018(4) 0.014(4) 0.016(4) C20 0.067(3) 0.063(4) 0.051(3) 0.018(3) -0.006(3) -0.004(3) C27 0.063(3) 0.068(4) 0.058(3) 0.022(3) -0.005(3) -0.007(3) C28 0.088(4) 0.081(5) 0.088(4) 0.037(4) -0.010(4) -0.009(4) C29 0.158(8) 0.100(6) 0.094(5) 0.052(5) 0.003(5) -0.026(6) C30 0.129(7) 0.071(5) 0.153(7) 0.039(5) 0.001(6) -0.032(5) C31 0.088(5) 0.088(5) 0.118(6) 0.020(5) 0.000(4) -0.029(4) C32 0.085(4) 0.077(5) 0.082(4) 0.011(3) -0.001(3) -0.015(4) C33 0.095(5) 0.165(8) 0.115(6) 0.075(6) 0.011(5) -0.006(5) C34 0.061(4) 0.078(5) 0.097(4) 0.006(3) 0.022(3) -0.011(3) C35 0.079(4) 0.095(6) 0.112(5) 0.027(4) -0.024(4) 0.014(4) C36 0.070(4) 0.121(6) 0.077(4) 0.010(4) -0.021(3) 0.001(4) _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 Ti1 N2 1.866(4) . ? Ti1 N1 1.879(5) . ? Ti1 N4 1.902(4) . ? Ti1 N3 1.926(5) . ? P1 N1 1.553(4) . ? P1 C14 1.829(8) . ? P1 C8 1.845(5) . ? P1 C7 1.850(6) . ? P2 N2 1.567(4) . ? P2 C27 1.839(5) . ? P2 C21 1.843(6) . ? P2 C20 1.855(5) . ? N3 C34 1.418(7) . ? N3 C33 1.428(8) . ? N4 C35 1.456(8) . ? N4 C36 1.465(7) . ? C1 C2 1.395(7) . ? C1 C6 1.397(7) . ? C2 C3 1.388(8) . ? C2 C7 1.501(8) . ? C3 C4 1.369(8) . ? C4 C5 1.379(8) . ? C5 C6 1.395(7) . ? C6 C20 1.500(7) . ? C8 C13 1.524(8) . ? C8 C9 1.524(8) . ? C9 C10 1.549(9) . ? C10 C11 1.452(10) . ? C11 C12 1.539(10) . ? C12 C13 1.549(8) . ? C14 C19A 1.170(18) . ? C14 C15 1.378(14) . ? C14 C19 1.568(15) . ? C14 C15A 1.735(16) . ? C15 C16 1.61(2) . ? C15A C19 1.371(19) . ? C15A C16A 1.71(2) . ? C16 C18A 1.60(3) . ? C16 C17 1.721(19) . ? C16 C16A 2.02(2) . ? C16A C17 1.216(19) . ? C16A C18 1.86(3) . ? C17 C18 1.223(16) . ? C17 C18A 1.56(2) . ? C18 C18A 1.64(2) . ? C18 C19 1.69(2) . ? C18A C19A 1.77(3) . ? C19 C19A 1.57(2) . ? C21 C22A 1.347(19) . ? C21 C22 1.487(10) . ? C21 C26 1.588(11) . ? C21 C26A 1.60(2) . ? C22 C23 1.618(13) . ? C22A C23A 1.61(3) . ? C23 C24 1.494(14) . ? C23 C23A 1.88(3) . ? C23A C24A 1.43(3) . ? C23A C25 2.00(3) . ? C24 C25A 0.90(4) . ? C24 C24A 1.28(2) . ? C24 C25 1.567(16) . ? C24A C25 0.90(2) . ? C24A C25A 1.51(4) . ? C25 C25A 1.22(3) . ? C25 C26 1.614(13) . ? C25 C26A 1.94(3) . ? C25A C26A 1.65(4) . ? C25A C26 1.93(4) . ? C26 C26A 0.88(2) . ? C27 C32 1.529(8) . ? C27 C28 1.529(8) . ? C28 C29 1.571(9) . ? C29 C30 1.484(10) . ? C30 C31 1.498(10) . ? C31 C32 1.532(9) . ? 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 N2 Ti1 N1 115.61(18) . . ? N2 Ti1 N4 109.68(18) . . ? N1 Ti1 N4 109.08(19) . . ? N2 Ti1 N3 109.65(19) . . ? N1 Ti1 N3 109.64(19) . . ? N4 Ti1 N3 102.3(2) . . ? N1 P1 C14 113.6(3) . . ? N1 P1 C8 113.5(3) . . ? C14 P1 C8 107.9(3) . . ? N1 P1 C7 113.0(2) . . ? C14 P1 C7 103.8(3) . . ? C8 P1 C7 104.2(3) . . ? N2 P2 C27 113.6(2) . . ? N2 P2 C21 113.5(2) . . ? C27 P2 C21 109.8(3) . . ? N2 P2 C20 114.6(2) . . ? C27 P2 C20 102.1(3) . . ? C21 P2 C20 102.2(2) . . ? P1 N1 Ti1 151.3(3) . . ? P2 N2 Ti1 157.7(3) . . ? C34 N3 C33 111.2(5) . . ? C34 N3 Ti1 119.5(4) . . ? C33 N3 Ti1 129.2(4) . . ? C35 N4 C36 112.2(5) . . ? C35 N4 Ti1 124.2(4) . . ? C36 N4 Ti1 123.5(4) . . ? C2 C1 C6 122.7(5) . . ? C3 C2 C1 116.6(5) . . ? C3 C2 C7 124.0(5) . . ? C1 C2 C7 119.4(5) . . ? C4 C3 C2 122.0(5) . . ? C3 C4 C5 120.8(5) . . ? C4 C5 C6 119.8(5) . . ? C5 C6 C1 118.1(5) . . ? C5 C6 C20 122.5(5) . . ? C1 C6 C20 119.4(4) . . ? C2 C7 P1 112.4(4) . . ? C13 C8 C9 110.8(5) . . ? C13 C8 P1 112.2(4) . . ? C9 C8 P1 116.9(4) . . ? C8 C9 C10 109.8(6) . . ? C11 C10 C9 114.2(6) . . ? C10 C11 C12 108.3(6) . . ? C11 C12 C13 112.1(6) . . ? C8 C13 C12 110.6(6) . . ? C19A C14 C15 109.2(12) . . ? C19A C14 C19 68.1(10) . . ? C15 C14 C19 117.8(9) . . ? C19A C14 C15A 110.6(11) . . ? C15 C14 C15A 82.2(8) . . ? C19 C14 C15A 48.7(7) . . ? C19A C14 P1 119.3(11) . . ? C15 C14 P1 122.0(8) . . ? C19 C14 P1 108.7(6) . . ? C15A C14 P1 106.7(6) . . ? C14 C15 C16 115.7(11) . . ? C19 C15A C16A 100.4(13) . . ? C19 C15A C14 59.2(8) . . ? C16A C15A C14 109.5(10) . . ? C18A C16 C15 96.9(14) . . ? C18A C16 C17 55.9(10) . . ? C15 C16 C17 108.3(11) . . ? C18A C16 C16A 85.1(13) . . ? C15 C16 C16A 83.9(10) . . ? C17 C16 C16A 36.9(7) . . ? C17 C16A C15A 112.5(16) . . ? C17 C16A C18 40.3(9) . . ? C15A C16A C18 79.3(11) . . ? C17 C16A C16 58.1(11) . . ? C15A C16A C16 94.9(11) . . ? C18 C16A C16 81.9(10) . . ? C16A C17 C18 99.7(15) . . ? C16A C17 C18A 125.0(16) . . ? C18 C17 C18A 71.2(12) . . ? C16A C17 C16 85.0(13) . . ? C18 C17 C16 119.0(12) . . ? C18A C17 C16 58.1(10) . . ? C17 C18 C18A 64.0(11) . . ? C17 C18 C19 114.8(13) . . ? C18A C18 C19 93.3(12) . . ? C17 C18 C16A 40.0(9) . . ? C18A C18 C16A 89.2(13) . . ? C19 C18 C16A 83.8(10) . . ? C17 C18A C16 66.0(12) . . ? C17 C18A C18 44.9(9) . . ? C16 C18A C18 103.7(15) . . ? C17 C18A C19A 111.2(15) . . ? C16 C18A C19A 99.2(15) . . ? C18 C18A C19A 82.4(13) . . ? C15A C19 C19A 110.0(13) . . ? C15A C19 C14 72.0(10) . . ? C19A C19 C14 43.8(7) . . ? C15A C19 C18 96.1(12) . . ? C19A C19 C18 87.4(11) . . ? C14 C19 C18 112.5(10) . . ? C14 C19A C19 68.1(11) . . ? C14 C19A C18A 111.1(15) . . ? C19 C19A C18A 92.7(13) . . ? C6 C20 P2 112.4(3) . . ? C22A C21 C22 106.8(10) . . ? C22A C21 C26 88.8(9) . . ? C22 C21 C26 114.6(6) . . ? C22A C21 C26A 114.9(12) . . ? C22 C21 C26A 88.2(10) . . ? C26 C21 C26A 32.2(8) . . ? C22A C21 P2 123.6(9) . . ? C22 C21 P2 113.1(5) . . ? C26 C21 P2 107.9(5) . . ? C26A C21 P2 104.7(9) . . ? C21 C22 C23 109.0(7) . . ? C21 C22A C23A 114.0(15) . . ? C24 C23 C22 108.3(9) . . ? C24 C23 C23A 80.1(10) . . ? C22 C23 C23A 97.9(10) . . ? C24A C23A C22A 108(2) . . ? C24A C23A C23 76.2(16) . . ? C22A C23A C23 96.4(14) . . ? C24A C23A C25 23.6(12) . . ? C22A C23A C25 84.8(14) . . ? C23 C23A C25 81.9(11) . . ? C25A C24 C24A 86(3) . . ? C25A C24 C23 124(3) . . ? C24A C24 C23 95.9(14) . . ? C25A C24 C25 51(2) . . ? C24A C24 C25 35.0(11) . . ? C23 C24 C25 112.2(9) . . ? C25 C24A C24 90(2) . . ? C25 C24A C23A 117(3) . . ? C24 C24A C23A 108(2) . . ? C25 C24A C25A 54(2) . . ? C24 C24A C25A 36.5(15) . . ? C23A C24A C25A 123(2) . . ? C24A C25 C25A 90(3) . . ? C24A C25 C24 54.9(17) . . ? C25A C25 C24 35.0(18) . . ? C24A C25 C26 132(2) . . ? C25A C25 C26 84.7(18) . . ? C24 C25 C26 106.5(9) . . ? C24A C25 C26A 122(2) . . ? C25A C25 C26A 57.9(18) . . ? C24 C25 C26A 81.5(10) . . ? C26 C25 C26A 26.9(7) . . ? C24A C25 C23A 39.5(18) . . ? C25A C25 C23A 104(2) . . ? C24 C25 C23A 74.6(10) . . ? C26 C25 C23A 96.2(9) . . ? C26A C25 C23A 99.2(11) . . ? C24 C25A C25 94(3) . . ? C24 C25A C24A 58(2) . . ? C25 C25A C24A 36.5(14) . . ? C24 C25A C26A 126(3) . . ? C25 C25A C26A 84(2) . . ? C24A C25A C26A 107(2) . . ? C24 C25A C26 124(3) . . ? C25 C25A C26 56.4(16) . . ? C24A C25A C26 84(2) . . ? C26A C25A C26 27.2(10) . . ? C26A C26 C21 74.8(17) . . ? C26A C26 C25 97.5(17) . . ? C21 C26 C25 109.2(7) . . ? C26A C26 C25A 58.8(18) . . ? C21 C26 C25A 99.9(12) . . ? C25 C26 C25A 38.9(10) . . ? C26 C26A C21 73.0(18) . . ? C26 C26A C25A 94(2) . . ? C21 C26A C25A 112.1(18) . . ? C26 C26A C25 55.6(15) . . ? C21 C26A C25 94.5(12) . . ? C25A C26A C25 38.6(13) . . ? C32 C27 C28 110.7(5) . . ? C32 C27 P2 117.0(4) . . ? C28 C27 P2 113.1(4) . . ? C27 C28 C29 109.2(5) . . ? C30 C29 C28 111.7(6) . . ? C29 C30 C31 111.0(6) . . ? C30 C31 C32 112.3(6) . . ? C27 C32 C31 110.4(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.575 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.070 #===end data_m-C6H4(CH2(t-Bu2)PN)2TiBr(NMe2) _database_code_CSD 215284 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_formula_sum 'C38 H62 Br N3 P2 Ti' _chemical_formula_weight 750.66 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' N N 0.0061 0.0033 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.413(8) _cell_length_b 17.579(9) _cell_length_c 17.190(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.449(11) _cell_angle_gamma 90.00 _cell_volume 4236(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.191509 _exptl_absorpt_correction_T_max 0.256635 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 17553 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6034 _reflns_number_gt 3638 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1582P)^2^+0.9476P] 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_number_reflns 6034 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2366 _refine_ls_wR_factor_gt 0.2067 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.006 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 Ti1 Ti 0.11902(7) 0.13317(5) 0.34726(6) 0.0412(3) Uani 1 1 d . . . Br1 Br -0.05976(7) 0.14454(6) 0.32271(7) 0.1117(4) Uani 1 1 d . . . N1 N 0.1553(3) 0.0398(2) 0.3888(3) 0.0470(12) Uani 1 1 d . . . N2 N 0.1700(4) 0.2156(3) 0.4068(3) 0.0516(13) Uani 1 1 d . . . N3 N 0.1437(4) 0.1397(3) 0.2433(3) 0.0559(13) Uani 1 1 d . . . P1 P 0.20017(11) -0.03441(8) 0.43408(9) 0.0417(4) Uani 1 1 d . . . P2 P 0.21019(11) 0.28083(8) 0.46779(9) 0.0472(4) Uani 1 1 d . . . C1 C 0.1141(5) -0.1144(3) 0.4052(4) 0.0589(17) Uani 1 1 d . . . C2 C 0.0890(6) -0.1245(4) 0.3147(4) 0.082(2) Uani 1 1 d . . . H2A H 0.0449 -0.1659 0.3005 0.123 Uiso 1 1 calc R . . H2B H 0.1460 -0.1354 0.2968 0.123 Uiso 1 1 calc R . . H2C H 0.0605 -0.0787 0.2897 0.123 Uiso 1 1 calc R . . C3 C 0.1495(6) -0.1899(4) 0.4468(6) 0.094(3) Uani 1 1 d . . . H3A H 0.1023 -0.2287 0.4293 0.141 Uiso 1 1 calc R . . H3B H 0.1602 -0.1837 0.5036 0.141 Uiso 1 1 calc R . . H3C H 0.2080 -0.2044 0.4333 0.141 Uiso 1 1 calc R . . C4 C 0.0217(5) -0.0911(4) 0.4297(5) 0.082(2) Uani 1 1 d . . . H4A H -0.0248 -0.1309 0.4156 0.123 Uiso 1 1 calc R . . H4B H -0.0029 -0.0451 0.4024 0.123 Uiso 1 1 calc R . . H4C H 0.0353 -0.0828 0.4865 0.123 Uiso 1 1 calc R . . C5 C 0.3219(4) -0.0533(3) 0.4152(4) 0.0548(16) Uani 1 1 d . . . C6 C 0.3785(6) -0.1137(5) 0.4707(6) 0.095(3) Uani 1 1 d . . . H6A H 0.4392 -0.1211 0.4579 0.143 Uiso 1 1 calc R . . H6B H 0.3436 -0.1607 0.4638 0.143 Uiso 1 1 calc R . . H6C H 0.3881 -0.0971 0.5252 0.143 Uiso 1 1 calc R . . C7 C 0.3766(5) 0.0217(4) 0.4283(4) 0.074(2) Uani 1 1 d . . . H7A H 0.4390 0.0145 0.4187 0.111 Uiso 1 1 calc R . . H7B H 0.3823 0.0385 0.4823 0.111 Uiso 1 1 calc R . . H7C H 0.3428 0.0593 0.3920 0.111 Uiso 1 1 calc R . . C8 C 0.3106(5) -0.0760(5) 0.3266(4) 0.093(3) Uani 1 1 d . . . H8A H 0.3723 -0.0857 0.3166 0.139 Uiso 1 1 calc R . . H8B H 0.2804 -0.0353 0.2928 0.139 Uiso 1 1 calc R . . H8C H 0.2721 -0.1210 0.3155 0.139 Uiso 1 1 calc R . . C9 C 0.2178(5) -0.0284(3) 0.5445(3) 0.0555(16) Uani 1 1 d . . . H9A H 0.1558 -0.0309 0.5574 0.067 Uiso 1 1 calc R . . H9B H 0.2538 -0.0726 0.5682 0.067 Uiso 1 1 calc R . . C10 C 0.2679(4) 0.0410(3) 0.5825(3) 0.0471(14) Uani 1 1 d . . . C11 C 0.3569(5) 0.0379(4) 0.6355(3) 0.0610(18) Uani 1 1 d . . . H11A H 0.3878 -0.0086 0.6472 0.073 Uiso 1 1 calc R . . C12 C 0.3990(5) 0.1031(5) 0.6705(4) 0.070(2) Uani 1 1 d . . . H12A H 0.4573 0.0997 0.7074 0.085 Uiso 1 1 calc R . . C13 C 0.3582(5) 0.1728(4) 0.6528(3) 0.0607(17) Uani 1 1 d . . . H13A H 0.3891 0.2161 0.6770 0.073 Uiso 1 1 calc R . . C14 C 0.2695(4) 0.1791(3) 0.5982(3) 0.0478(14) Uani 1 1 d . . . C15 C 0.2256(4) 0.1128(3) 0.5660(3) 0.0452(14) Uani 1 1 d . . . H15A H 0.1653 0.1158 0.5319 0.054 Uiso 1 1 calc R . . C16 C 0.2214(5) 0.2541(3) 0.5746(3) 0.0562(16) Uani 1 1 d . . . H16A H 0.2572 0.2935 0.6082 0.067 Uiso 1 1 calc R . . H16B H 0.1582 0.2525 0.5850 0.067 Uiso 1 1 calc R . . C17 C 0.3343(5) 0.3097(4) 0.4598(4) 0.0615(17) Uani 1 1 d . . . C18 C 0.3287(7) 0.3523(5) 0.3824(5) 0.097(3) Uani 1 1 d . . . H18A H 0.3917 0.3671 0.3788 0.146 Uiso 1 1 calc R . . H18B H 0.2898 0.3968 0.3812 0.146 Uiso 1 1 calc R . . H18C H 0.3011 0.3200 0.3381 0.146 Uiso 1 1 calc R . . C19 C 0.3875(6) 0.3571(5) 0.5318(5) 0.097(3) Uani 1 1 d . . . H19A H 0.4494 0.3706 0.5245 0.146 Uiso 1 1 calc R . . H19B H 0.3943 0.3278 0.5799 0.146 Uiso 1 1 calc R . . H19C H 0.3518 0.4025 0.5358 0.146 Uiso 1 1 calc R . . C20 C 0.3898(5) 0.2354(4) 0.4587(5) 0.086(2) Uani 1 1 d . . . H20A H 0.4535 0.2469 0.4545 0.129 Uiso 1 1 calc R . . H20B H 0.3585 0.2052 0.4138 0.129 Uiso 1 1 calc R . . H20C H 0.3921 0.2078 0.5073 0.129 Uiso 1 1 calc R . . C21 C 0.1232(6) 0.3621(3) 0.4524(4) 0.069(2) Uani 1 1 d . . . C22 C 0.1616(6) 0.4344(4) 0.4994(5) 0.086(2) Uani 1 1 d . . . H22A H 0.1133 0.4731 0.4893 0.128 Uiso 1 1 calc R . . H22B H 0.2169 0.4522 0.4826 0.128 Uiso 1 1 calc R . . H22C H 0.1787 0.4231 0.5555 0.128 Uiso 1 1 calc R . . C23 C 0.0322(5) 0.3349(4) 0.4794(5) 0.086(2) Uani 1 1 d . . . H23A H -0.0132 0.3757 0.4730 0.129 Uiso 1 1 calc R . . H23B H 0.0496 0.3199 0.5346 0.129 Uiso 1 1 calc R . . H23C H 0.0044 0.2924 0.4472 0.129 Uiso 1 1 calc R . . C24 C 0.0942(7) 0.3795(4) 0.3608(4) 0.097(3) Uani 1 1 d . . . H24A H 0.0497 0.4210 0.3512 0.146 Uiso 1 1 calc R . . H24B H 0.0651 0.3352 0.3326 0.146 Uiso 1 1 calc R . . H24C H 0.1500 0.3930 0.3424 0.146 Uiso 1 1 calc R . . C25 C 0.1452(7) 0.0756(4) 0.1888(4) 0.086(2) Uani 1 1 d . . . H25A H 0.1592 0.0940 0.1402 0.130 Uiso 1 1 calc R . . H25B H 0.0841 0.0510 0.1768 0.130 Uiso 1 1 calc R . . H25C H 0.1934 0.0399 0.2138 0.130 Uiso 1 1 calc R . . C26 C 0.1539(7) 0.2103(4) 0.2031(4) 0.100(3) Uani 1 1 d . . . H26A H 0.1659 0.1995 0.1515 0.150 Uiso 1 1 calc R . . H26B H 0.2062 0.2388 0.2344 0.150 Uiso 1 1 calc R . . H26C H 0.0962 0.2394 0.1965 0.150 Uiso 1 1 calc R . . C27 C -0.4358(17) 0.2001(9) 0.2948(9) 0.157(6) Uani 1 1 d . . . H27A H -0.4331 0.2410 0.3296 0.188 Uiso 1 1 calc R . . C28 C -0.5225(14) 0.1633(11) 0.2625(11) 0.157(6) Uani 1 1 d . . . H28A H -0.5789 0.1782 0.2756 0.189 Uiso 1 1 calc R . . C29 C -0.5200(14) 0.0984(8) 0.2057(9) 0.149(5) Uani 1 1 d . . . H29A H -0.5760 0.0734 0.1813 0.179 Uiso 1 1 calc R . . C30 C -0.4386(13) 0.0775(7) 0.1908(8) 0.124(4) Uani 1 1 d . . . H30A H -0.4344 0.0364 0.1577 0.149 Uiso 1 1 calc R . . C31 C -0.3645(14) 0.1168(8) 0.2244(9) 0.140(5) Uani 1 1 d . . . H31A H -0.3070 0.1031 0.2125 0.169 Uiso 1 1 calc R . . C32 C -0.3619(14) 0.1765(8) 0.2756(7) 0.140(5) Uani 1 1 d . . . H32A H -0.3039 0.2003 0.2968 0.168 Uiso 1 1 calc R . . C33 C -0.3064(19) 0.4361(13) 0.3004(8) 0.163(8) Uani 1 1 d . . . H33A H -0.2972 0.4550 0.2522 0.196 Uiso 1 1 calc R . . C34 C -0.3728(13) 0.4601(9) 0.3279(13) 0.143(6) Uani 1 1 d . . . H34A H -0.4131 0.4962 0.2980 0.172 Uiso 1 1 calc R . . C35 C -0.3899(8) 0.4402(9) 0.3912(15) 0.130(5) Uani 1 1 d . . . H35A H -0.4426 0.4606 0.4062 0.156 Uiso 1 1 calc R . . C36 C -0.3336(18) 0.3886(12) 0.4408(8) 0.155(7) Uani 1 1 d . . . H36A H -0.3449 0.3750 0.4901 0.186 Uiso 1 1 calc R . . C37 C -0.2585(13) 0.3580(7) 0.4129(13) 0.150(5) Uani 1 1 d . . . H37A H -0.2179 0.3223 0.4430 0.180 Uiso 1 1 calc R . . C38 C -0.2457(12) 0.3810(10) 0.3417(14) 0.144(5) Uani 1 1 d . . . H38A H -0.1974 0.3604 0.3206 0.173 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 Ti1 0.0466(6) 0.0361(6) 0.0366(6) 0.0004(4) 0.0011(5) -0.0010(4) Br1 0.0830(7) 0.1164(8) 0.1283(9) 0.0042(6) 0.0097(6) 0.0003(5) N1 0.062(3) 0.036(3) 0.041(3) 0.002(2) 0.008(2) 0.003(2) N2 0.069(3) 0.042(3) 0.039(3) -0.003(2) 0.000(2) -0.004(2) N3 0.075(4) 0.050(3) 0.040(3) 0.002(2) 0.007(3) -0.011(3) P1 0.0466(9) 0.0358(8) 0.0437(8) 0.0010(7) 0.0122(7) 0.0019(6) P2 0.0578(10) 0.0374(8) 0.0421(9) -0.0029(7) 0.0028(7) -0.0009(7) C1 0.065(4) 0.039(3) 0.078(5) -0.005(3) 0.027(4) -0.007(3) C2 0.084(6) 0.081(5) 0.078(5) -0.024(4) 0.013(4) -0.028(4) C3 0.100(6) 0.049(4) 0.134(7) 0.024(5) 0.026(5) -0.004(4) C4 0.059(5) 0.088(5) 0.106(6) -0.022(5) 0.031(4) -0.014(4) C5 0.047(4) 0.059(4) 0.060(4) -0.010(3) 0.016(3) 0.008(3) C6 0.067(5) 0.090(6) 0.121(7) 0.016(5) 0.009(5) 0.026(4) C7 0.061(5) 0.081(5) 0.086(5) -0.005(4) 0.029(4) -0.012(4) C8 0.069(5) 0.137(7) 0.079(5) -0.042(5) 0.032(4) 0.006(5) C9 0.074(4) 0.049(3) 0.043(3) 0.011(3) 0.014(3) 0.008(3) C10 0.056(4) 0.057(4) 0.029(3) 0.004(3) 0.013(3) 0.007(3) C11 0.070(5) 0.074(5) 0.036(3) 0.009(3) 0.007(3) 0.017(4) C12 0.057(4) 0.108(6) 0.038(4) 0.009(4) -0.007(3) 0.009(4) C13 0.066(4) 0.074(5) 0.037(3) -0.004(3) 0.002(3) -0.011(4) C14 0.057(4) 0.055(4) 0.032(3) -0.002(3) 0.012(3) -0.003(3) C15 0.050(4) 0.054(4) 0.033(3) 0.004(3) 0.012(3) 0.003(3) C16 0.071(4) 0.049(3) 0.047(4) -0.009(3) 0.012(3) -0.001(3) C17 0.065(4) 0.060(4) 0.058(4) -0.002(3) 0.014(3) -0.013(3) C18 0.103(7) 0.097(6) 0.094(6) 0.026(5) 0.028(5) -0.029(5) C19 0.071(5) 0.104(6) 0.108(7) -0.026(5) 0.003(5) -0.028(5) C20 0.072(5) 0.092(6) 0.102(6) 0.019(5) 0.037(5) 0.008(4) C21 0.088(5) 0.043(3) 0.064(4) -0.006(3) -0.007(4) 0.014(4) C22 0.110(6) 0.047(4) 0.093(6) -0.021(4) 0.010(5) 0.002(4) C23 0.066(5) 0.069(5) 0.117(7) -0.012(5) 0.008(5) 0.007(4) C24 0.127(7) 0.079(5) 0.066(5) 0.007(4) -0.018(5) 0.041(5) C25 0.122(7) 0.078(5) 0.057(4) 0.001(4) 0.016(4) -0.001(5) C26 0.166(9) 0.071(5) 0.062(5) 0.002(4) 0.027(5) -0.030(5) C27 0.22(2) 0.121(11) 0.121(11) -0.003(8) 0.016(13) 0.049(13) C28 0.177(15) 0.160(14) 0.148(13) 0.061(11) 0.066(11) 0.076(12) C29 0.203(17) 0.115(11) 0.117(10) 0.043(9) 0.010(10) -0.009(11) C30 0.184(14) 0.075(7) 0.123(9) 0.001(6) 0.051(10) -0.025(9) C31 0.242(19) 0.091(8) 0.117(10) 0.042(8) 0.101(11) 0.032(10) C32 0.210(17) 0.105(10) 0.099(9) 0.026(8) 0.026(9) -0.003(10) C33 0.20(2) 0.21(2) 0.086(8) -0.017(11) 0.037(11) -0.113(17) C34 0.122(13) 0.138(12) 0.149(15) 0.042(11) -0.009(9) -0.041(10) C35 0.084(8) 0.097(9) 0.212(18) -0.054(10) 0.038(11) -0.013(7) C36 0.208(18) 0.167(15) 0.111(10) -0.038(11) 0.078(12) -0.112(14) C37 0.153(14) 0.105(9) 0.171(14) 0.047(10) -0.006(11) -0.001(9) C38 0.133(12) 0.136(12) 0.180(16) -0.036(11) 0.068(12) -0.013(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. ; 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 Ti1 N1 1.818(4) . ? Ti1 N2 1.827(4) . ? Ti1 N3 1.905(5) . ? Ti1 Br1 2.5202(19) . ? N1 P1 1.578(5) . ? N2 P2 1.570(5) . ? N3 C26 1.444(8) . ? N3 C25 1.469(8) . ? P1 C9 1.859(6) . ? P1 C1 1.864(6) . ? P1 C5 1.887(6) . ? P2 C16 1.865(6) . ? P2 C21 1.878(7) . ? P2 C17 1.895(7) . ? C1 C2 1.524(10) . ? C1 C4 1.543(9) . ? C1 C3 1.537(9) . ? C5 C6 1.530(9) . ? C5 C7 1.525(9) . ? C5 C8 1.545(9) . ? C9 C10 1.488(8) . ? C10 C11 1.391(9) . ? C10 C15 1.402(8) . ? C11 C12 1.368(10) . ? C12 C13 1.362(10) . ? C13 C14 1.405(9) . ? C14 C15 1.380(8) . ? C14 C16 1.500(8) . ? C17 C18 1.512(10) . ? C17 C19 1.539(9) . ? C17 C20 1.534(10) . ? C21 C22 1.539(9) . ? C21 C24 1.562(10) . ? C21 C23 1.564(11) . ? C27 C32 1.257(18) . ? C27 C28 1.40(2) . ? C28 C29 1.51(2) . ? C29 C30 1.310(18) . ? C30 C31 1.290(18) . ? C31 C32 1.364(17) . ? C33 C34 1.24(2) . ? C33 C38 1.39(2) . ? C34 C35 1.221(18) . ? C35 C36 1.374(19) . ? C36 C37 1.39(2) . ? C37 C38 1.341(19) . ? 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 N1 Ti1 N2 117.1(2) . . ? N1 Ti1 N3 108.9(2) . . ? N2 Ti1 N3 109.8(2) . . ? N1 Ti1 Br1 109.10(16) . . ? N2 Ti1 Br1 107.03(17) . . ? N3 Ti1 Br1 104.16(17) . . ? P1 N1 Ti1 170.9(3) . . ? P2 N2 Ti1 172.3(3) . . ? C26 N3 C25 109.6(5) . . ? C26 N3 Ti1 124.3(4) . . ? C25 N3 Ti1 125.8(4) . . ? N1 P1 C9 113.6(3) . . ? N1 P1 C1 108.7(3) . . ? C9 P1 C1 103.8(3) . . ? N1 P1 C5 110.5(3) . . ? C9 P1 C5 105.9(3) . . ? C1 P1 C5 114.2(3) . . ? N2 P2 C16 114.0(3) . . ? N2 P2 C21 109.3(3) . . ? C16 P2 C21 103.5(3) . . ? N2 P2 C17 110.8(3) . . ? C16 P2 C17 105.7(3) . . ? C21 P2 C17 113.4(3) . . ? C2 C1 C4 107.2(6) . . ? C2 C1 C3 110.4(6) . . ? C4 C1 C3 108.4(6) . . ? C2 C1 P1 110.2(4) . . ? C4 C1 P1 106.9(4) . . ? C3 C1 P1 113.5(5) . . ? C6 C5 C7 109.0(6) . . ? C6 C5 C8 110.7(6) . . ? C7 C5 C8 107.5(6) . . ? C6 C5 P1 113.4(5) . . ? C7 C5 P1 107.0(4) . . ? C8 C5 P1 109.0(4) . . ? C10 C9 P1 115.5(4) . . ? C11 C10 C15 117.3(6) . . ? C11 C10 C9 122.3(6) . . ? C15 C10 C9 120.4(5) . . ? C12 C11 C10 120.2(6) . . ? C13 C12 C11 122.0(6) . . ? C12 C13 C14 120.0(6) . . ? C15 C14 C13 117.5(6) . . ? C15 C14 C16 119.6(5) . . ? C13 C14 C16 122.8(6) . . ? C14 C15 C10 122.9(5) . . ? C14 C16 P2 114.6(4) . . ? C18 C17 C19 110.7(6) . . ? C18 C17 C20 109.4(6) . . ? C19 C17 C20 107.9(6) . . ? C18 C17 P2 109.8(5) . . ? C19 C17 P2 112.9(5) . . ? C20 C17 P2 106.1(5) . . ? C22 C21 C24 110.2(6) . . ? C22 C21 C23 108.7(6) . . ? C24 C21 C23 108.2(7) . . ? C22 C21 P2 114.0(5) . . ? C24 C21 P2 107.7(5) . . ? C23 C21 P2 107.7(5) . . ? C32 C27 C28 118.4(17) . . ? C27 C28 C29 116.8(15) . . ? C30 C29 C28 119.8(15) . . ? C29 C30 C31 116.6(15) . . ? C30 C31 C32 126.6(16) . . ? C27 C32 C31 121.7(18) . . ? C34 C33 C38 119.7(16) . . ? C35 C34 C33 125.3(18) . . ? C34 C35 C36 122.0(15) . . ? C35 C36 C37 115.8(12) . . ? C38 C37 C36 118.8(14) . . ? C37 C38 C33 118.3(15) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.574 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.085 #===end data_m-C6H4(CH2(t-Bu2)PN)2TiBz2 _database_code_CSD 215285 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C44 H64 N2 P2 Ti' _chemical_formula_weight 730.81 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' N N 0.0061 0.0033 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.799(3) _cell_length_b 14.917(6) _cell_length_c 29.534(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4317(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.110941 _exptl_absorpt_correction_T_max 0.152547 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8129 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1590 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5712 _reflns_number_gt 2985 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0367P)^2^+4.8319P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(7) _refine_ls_number_reflns 5712 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1801 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.004 _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 Ti1 Ti 0.97127(15) 0.70719(10) 0.11961(5) 0.0447(5) Uani 1 1 d . . . P1 P 1.2384(3) 0.67041(18) 0.18945(8) 0.0487(7) Uani 1 1 d . . . P2 P 1.0111(3) 0.90128(16) 0.06223(8) 0.0533(7) Uani 1 1 d . . . N1 N 1.1118(7) 0.6767(5) 0.1575(2) 0.049(2) Uani 1 1 d . . . N2 N 0.9881(7) 0.8093(5) 0.0873(2) 0.057(2) Uani 1 1 d . . . C1 C 1.3870(8) 0.8055(6) 0.1432(3) 0.044(2) Uani 1 1 d . . . C2 C 1.4599(10) 0.8775(8) 0.1614(3) 0.058(3) Uani 1 1 d . . . H2A H 1.5161 0.8676 0.1862 0.069 Uiso 1 1 calc R . . C3 C 1.4511(10) 0.9608(8) 0.1439(4) 0.068(3) Uani 1 1 d . . . H3A H 1.5020 1.0075 0.1562 0.082 Uiso 1 1 calc R . . C4 C 1.3645(10) 0.9763(6) 0.1071(4) 0.061(3) Uani 1 1 d . . . H4A H 1.3581 1.0336 0.0948 0.074 Uiso 1 1 calc R . . C5 C 1.2888(9) 0.9076(8) 0.0888(3) 0.049(3) Uani 1 1 d . . . C6 C 1.3041(8) 0.8223(6) 0.1060(3) 0.046(3) Uani 1 1 d . . . H6A H 1.2579 0.7750 0.0925 0.055 Uiso 1 1 calc R . . C7 C 1.3948(8) 0.7113(7) 0.1626(3) 0.061(3) Uani 1 1 d . . . H7A H 1.4678 0.7096 0.1847 0.074 Uiso 1 1 calc R . . H7B H 1.4190 0.6704 0.1383 0.074 Uiso 1 1 calc R . . C8 C 1.2146(11) 0.7376(8) 0.2429(3) 0.069(3) Uani 1 1 d . . . C9 C 1.1448(10) 0.8254(7) 0.2282(4) 0.087(4) Uani 1 1 d . . . H9A H 1.1315 0.8631 0.2542 0.131 Uiso 1 1 calc R . . H9B H 1.0580 0.8120 0.2147 0.131 Uiso 1 1 calc R . . H9C H 1.2013 0.8559 0.2066 0.131 Uiso 1 1 calc R . . C10 C 1.1125(10) 0.6878(7) 0.2733(3) 0.084(4) Uani 1 1 d . . . H10A H 1.0993 0.7210 0.3008 0.127 Uiso 1 1 calc R . . H10B H 1.1475 0.6293 0.2803 0.127 Uiso 1 1 calc R . . H10C H 1.0270 0.6820 0.2577 0.127 Uiso 1 1 calc R . . C11 C 1.3457(10) 0.7561(9) 0.2672(3) 0.108(5) Uani 1 1 d . . . H11A H 1.3275 0.7913 0.2938 0.162 Uiso 1 1 calc R . . H11B H 1.4063 0.7884 0.2476 0.162 Uiso 1 1 calc R . . H11C H 1.3873 0.7004 0.2760 0.162 Uiso 1 1 calc R . . C12 C 1.2780(12) 0.5492(7) 0.2016(4) 0.069(3) Uani 1 1 d . . . C13 C 1.1399(11) 0.5017(7) 0.2124(4) 0.086(4) Uani 1 1 d . . . H13A H 1.1562 0.4394 0.2184 0.129 Uiso 1 1 calc R . . H13B H 1.0797 0.5074 0.1869 0.129 Uiso 1 1 calc R . . H13C H 1.0988 0.5291 0.2384 0.129 Uiso 1 1 calc R . . C14 C 1.3812(11) 0.5361(8) 0.2403(4) 0.113(5) Uani 1 1 d . . . H14A H 1.3982 0.4732 0.2444 0.170 Uiso 1 1 calc R . . H14B H 1.3448 0.5609 0.2677 0.170 Uiso 1 1 calc R . . H14C H 1.4651 0.5659 0.2328 0.170 Uiso 1 1 calc R . . C15 C 1.3355(11) 0.5086(7) 0.1587(4) 0.097(4) Uani 1 1 d . . . H15A H 1.3569 0.4467 0.1638 0.145 Uiso 1 1 calc R . . H15B H 1.4168 0.5402 0.1501 0.145 Uiso 1 1 calc R . . H15C H 1.2691 0.5132 0.1349 0.145 Uiso 1 1 calc R . . C16 C 1.1929(8) 0.9223(6) 0.0493(3) 0.054(3) Uani 1 1 d . . . H16A H 1.2203 0.8833 0.0247 0.065 Uiso 1 1 calc R . . H16B H 1.2026 0.9837 0.0390 0.065 Uiso 1 1 calc R . . C17 C 0.9530(12) 0.9979(7) 0.0976(4) 0.076(3) Uani 1 1 d . . . C18 C 0.7944(11) 0.9980(8) 0.1023(4) 0.114(5) Uani 1 1 d . . . H18A H 0.7665 1.0483 0.1203 0.171 Uiso 1 1 calc R . . H18B H 0.7654 0.9435 0.1167 0.171 Uiso 1 1 calc R . . H18C H 0.7536 1.0023 0.0728 0.171 Uiso 1 1 calc R . . C19 C 1.0012(15) 1.0883(7) 0.0803(4) 0.140(5) Uani 1 1 d . . . H19A H 0.9662 1.1349 0.0994 0.209 Uiso 1 1 calc R . . H19B H 0.9686 1.0971 0.0499 0.209 Uiso 1 1 calc R . . H19C H 1.0991 1.0901 0.0804 0.209 Uiso 1 1 calc R . . C20 C 1.0110(12) 0.9803(8) 0.1456(4) 0.106(4) Uani 1 1 d . . . H20A H 0.9832 1.0277 0.1656 0.158 Uiso 1 1 calc R . . H20B H 1.1088 0.9781 0.1443 0.158 Uiso 1 1 calc R . . H20C H 0.9768 0.9242 0.1568 0.158 Uiso 1 1 calc R . . C21 C 0.9272(11) 0.8972(8) 0.0055(3) 0.072(3) Uani 1 1 d . . . C22 C 0.7775(12) 0.8655(9) 0.0107(4) 0.131(6) Uani 1 1 d . . . H22A H 0.7353 0.8626 -0.0186 0.197 Uiso 1 1 calc R . . H22B H 0.7285 0.9071 0.0294 0.197 Uiso 1 1 calc R . . H22C H 0.7759 0.8072 0.0245 0.197 Uiso 1 1 calc R . . C23 C 0.9304(14) 0.9859(8) -0.0207(3) 0.119(5) Uani 1 1 d . . . H23A H 0.8874 0.9779 -0.0496 0.179 Uiso 1 1 calc R . . H23B H 1.0234 1.0043 -0.0251 0.179 Uiso 1 1 calc R . . H23C H 0.8825 1.0311 -0.0039 0.179 Uiso 1 1 calc R . . C24 C 1.0042(12) 0.8233(7) -0.0225(3) 0.092(4) Uani 1 1 d . . . H24A H 0.9647 0.8190 -0.0522 0.138 Uiso 1 1 calc R . . H24B H 0.9962 0.7666 -0.0074 0.138 Uiso 1 1 calc R . . H24C H 1.0989 0.8391 -0.0251 0.138 Uiso 1 1 calc R . . C25 C 0.9439(10) 0.6043(6) 0.0684(3) 0.063(3) Uani 1 1 d . . . H25A H 0.8754 0.6249 0.0471 0.076 Uiso 1 1 calc R . . H25B H 1.0289 0.5981 0.0518 0.076 Uiso 1 1 calc R . . C26 C 0.9044(13) 0.5179(8) 0.0843(3) 0.064(3) Uani 1 1 d . . . C27 C 0.9947(13) 0.4491(9) 0.0952(4) 0.088(4) Uani 1 1 d . . . H27A H 1.0876 0.4596 0.0916 0.106 Uiso 1 1 calc R . . C28 C 0.9537(17) 0.3662(9) 0.1112(5) 0.108(5) Uani 1 1 d . . . H28A H 1.0193 0.3228 0.1172 0.129 Uiso 1 1 calc R . . C29 C 0.8242(18) 0.3471(9) 0.1180(5) 0.111(5) Uani 1 1 d . . . H29A H 0.7981 0.2915 0.1293 0.133 Uiso 1 1 calc R . . C30 C 0.7299(14) 0.4106(10) 0.1081(4) 0.101(4) Uani 1 1 d . . . H30A H 0.6376 0.3979 0.1118 0.121 Uiso 1 1 calc R . . C31 C 0.7695(15) 0.4944(8) 0.0925(4) 0.098(4) Uani 1 1 d . . . H31A H 0.7022 0.5372 0.0873 0.117 Uiso 1 1 calc R . . C32 C 0.7792(8) 0.7148(7) 0.1531(3) 0.066(3) Uani 1 1 d . . . H32A H 0.7464 0.7757 0.1492 0.079 Uiso 1 1 calc R . . H32B H 0.7171 0.6763 0.1365 0.079 Uiso 1 1 calc R . . C33 C 0.7630(9) 0.6925(7) 0.2017(3) 0.055(3) Uani 1 1 d . . . C34 C 0.7599(9) 0.6046(7) 0.2174(4) 0.059(3) Uani 1 1 d . . . H34A H 0.7667 0.5578 0.1967 0.071 Uiso 1 1 calc R . . C35 C 0.7471(11) 0.5848(8) 0.2632(4) 0.079(3) Uani 1 1 d . . . H35A H 0.7469 0.5253 0.2726 0.095 Uiso 1 1 calc R . . C36 C 0.7349(11) 0.6505(9) 0.2943(4) 0.077(3) Uani 1 1 d . . . H36A H 0.7228 0.6365 0.3247 0.093 Uiso 1 1 calc R . . C37 C 0.7403(12) 0.7373(8) 0.2807(4) 0.075(3) Uani 1 1 d . . . H37A H 0.7349 0.7829 0.3021 0.090 Uiso 1 1 calc R . . C38 C 0.7541(10) 0.7590(7) 0.2346(4) 0.063(3) Uani 1 1 d . . . H38A H 0.7573 0.8189 0.2260 0.076 Uiso 1 1 calc R . . C39 C 0.283(2) 0.249(2) 0.0403(12) 0.194(14) Uani 1 1 d . . . H39A H 0.1981 0.2733 0.0335 0.233 Uiso 1 1 calc R . . C40 C 0.340(3) 0.2693(11) 0.0797(9) 0.151(7) Uani 1 1 d . . . H40A H 0.2959 0.3076 0.0998 0.182 Uiso 1 1 calc R . . C41 C 0.457(3) 0.2355(17) 0.0896(7) 0.145(7) Uani 1 1 d . . . H41A H 0.4965 0.2488 0.1174 0.174 Uiso 1 1 calc R . . C42 C 0.521(2) 0.1822(19) 0.0610(14) 0.209(17) Uani 1 1 d . . . H42A H 0.6083 0.1598 0.0665 0.251 Uiso 1 1 calc R . . C43 C 0.450(6) 0.163(2) 0.0231(11) 0.29(4) Uani 1 1 d . . . H43A H 0.4909 0.1201 0.0048 0.343 Uiso 1 1 calc R . . C44 C 0.343(6) 0.192(4) 0.0085(13) 0.33(4) Uani 1 1 d . . . H44A H 0.3068 0.1779 -0.0197 0.396 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 Ti1 0.0363(10) 0.0535(10) 0.0442(10) 0.0026(9) -0.0042(9) -0.0057(9) P1 0.0337(16) 0.0644(18) 0.0481(16) 0.0044(14) -0.0026(15) 0.0008(13) P2 0.052(2) 0.0533(16) 0.0543(16) 0.0068(13) -0.0092(15) -0.0021(15) N1 0.037(4) 0.061(5) 0.048(5) 0.005(4) -0.010(4) -0.001(4) N2 0.052(5) 0.066(5) 0.053(4) 0.010(4) -0.011(4) 0.000(4) C1 0.019(5) 0.059(7) 0.055(7) -0.014(6) 0.012(5) -0.009(5) C2 0.037(7) 0.090(9) 0.045(6) -0.001(6) -0.007(5) -0.009(7) C3 0.044(8) 0.082(9) 0.078(8) -0.022(7) -0.007(7) -0.020(7) C4 0.042(7) 0.057(7) 0.085(9) 0.000(7) 0.014(7) -0.011(6) C5 0.029(6) 0.072(8) 0.046(6) -0.011(6) 0.006(5) -0.001(6) C6 0.024(6) 0.059(7) 0.055(7) -0.002(5) 0.001(5) -0.005(5) C7 0.040(6) 0.073(7) 0.070(7) 0.009(6) -0.008(5) -0.001(6) C8 0.045(8) 0.112(10) 0.049(7) -0.015(7) -0.003(6) -0.004(7) C9 0.074(8) 0.095(10) 0.092(9) -0.046(8) 0.018(7) -0.007(8) C10 0.073(8) 0.125(10) 0.055(7) -0.005(7) 0.030(6) -0.032(8) C11 0.050(8) 0.215(16) 0.060(8) -0.027(9) -0.008(7) -0.034(8) C12 0.075(9) 0.076(8) 0.057(7) 0.014(6) 0.003(7) 0.006(7) C13 0.084(9) 0.071(8) 0.102(10) 0.021(7) 0.016(7) -0.002(7) C14 0.080(9) 0.126(11) 0.133(12) 0.046(9) -0.039(9) 0.027(8) C15 0.104(11) 0.071(8) 0.114(11) 0.008(8) 0.024(8) 0.021(8) C16 0.049(7) 0.061(7) 0.053(7) 0.000(5) -0.009(5) -0.013(5) C17 0.068(9) 0.068(8) 0.093(9) 0.008(7) 0.026(7) 0.007(6) C18 0.065(9) 0.133(11) 0.145(13) -0.019(10) 0.009(8) 0.028(8) C19 0.181(14) 0.059(8) 0.178(13) -0.003(9) 0.042(13) 0.007(11) C20 0.097(10) 0.140(11) 0.080(8) -0.041(8) -0.012(9) 0.029(9) C21 0.069(9) 0.090(9) 0.058(7) 0.018(7) -0.022(6) -0.005(7) C22 0.079(10) 0.168(14) 0.146(13) 0.029(10) -0.070(10) -0.024(10) C23 0.172(15) 0.111(10) 0.075(9) 0.042(8) -0.025(9) 0.002(10) C24 0.094(9) 0.124(10) 0.058(7) -0.020(7) -0.016(7) -0.002(9) C25 0.069(8) 0.064(7) 0.056(7) -0.007(6) 0.002(6) -0.025(6) C26 0.072(9) 0.070(9) 0.051(7) -0.012(6) -0.007(7) -0.009(8) C27 0.063(9) 0.093(10) 0.108(10) -0.009(8) -0.007(8) -0.018(9) C28 0.120(13) 0.075(10) 0.127(12) 0.014(8) -0.036(12) 0.008(10) C29 0.143(15) 0.075(10) 0.115(11) 0.008(10) 0.010(13) -0.006(11) C30 0.093(11) 0.080(10) 0.130(12) -0.025(10) 0.022(9) -0.027(9) C31 0.099(11) 0.062(9) 0.132(11) 0.001(8) -0.030(10) -0.008(8) C32 0.021(6) 0.104(9) 0.072(7) 0.018(7) -0.003(6) 0.000(6) C33 0.032(6) 0.067(8) 0.067(8) -0.001(7) 0.001(6) -0.008(6) C34 0.045(7) 0.064(8) 0.069(8) -0.014(7) -0.001(6) -0.009(6) C35 0.071(8) 0.081(9) 0.086(10) 0.030(8) 0.008(8) -0.003(8) C36 0.073(9) 0.097(10) 0.062(8) 0.018(8) 0.004(7) -0.001(8) C37 0.084(9) 0.074(9) 0.067(8) -0.005(7) 0.017(8) -0.008(7) C38 0.049(7) 0.058(7) 0.082(9) 0.002(7) -0.001(7) -0.007(6) C39 0.118(17) 0.29(4) 0.17(2) 0.11(3) -0.07(2) -0.05(2) C40 0.15(2) 0.139(15) 0.17(2) 0.003(15) -0.009(16) 0.031(15) C41 0.110(16) 0.153(19) 0.172(19) 0.034(16) -0.055(18) -0.053(13) C42 0.113(17) 0.16(3) 0.35(5) 0.08(3) 0.14(3) 0.030(16) C43 0.55(10) 0.16(2) 0.15(3) -0.04(3) 0.18(5) -0.14(4) C44 0.47(8) 0.43(7) 0.09(2) 0.08(3) -0.05(3) -0.19(5) _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 Ti1 N2 1.805(7) . ? Ti1 N1 1.831(7) . ? Ti1 C32 2.129(8) . ? Ti1 C25 2.172(8) . ? P1 N1 1.562(7) . ? P1 C7 1.830(9) . ? P1 C8 1.883(10) . ? P1 C12 1.883(10) . ? P2 N2 1.576(7) . ? P2 C16 1.849(8) . ? P2 C21 1.866(9) . ? P2 C17 1.869(11) . ? C1 C6 1.388(11) . ? C1 C2 1.397(11) . ? C1 C7 1.519(12) . ? C2 C3 1.349(12) . ? C3 C4 1.399(12) . ? C4 C5 1.376(12) . ? C5 C6 1.379(12) . ? C5 C16 1.512(11) . ? C8 C11 1.498(12) . ? C8 C10 1.535(13) . ? C8 C9 1.541(13) . ? C12 C15 1.514(13) . ? C12 C14 1.538(13) . ? C12 C13 1.561(13) . ? C17 C19 1.517(13) . ? C17 C20 1.550(13) . ? C17 C18 1.561(13) . ? C21 C23 1.535(13) . ? C21 C22 1.549(14) . ? C21 C24 1.571(13) . ? C25 C26 1.427(13) . ? C26 C31 1.388(15) . ? C26 C27 1.392(13) . ? C27 C28 1.384(14) . ? C28 C29 1.316(15) . ? C29 C30 1.356(15) . ? C30 C31 1.388(14) . ? C32 C33 1.483(11) . ? C33 C38 1.391(12) . ? C33 C34 1.390(12) . ? C34 C35 1.392(12) . ? C35 C36 1.349(14) . ? C36 C37 1.356(13) . ? C37 C38 1.405(12) . ? C39 C40 1.33(2) . ? C39 C44 1.40(6) . ? C40 C41 1.28(2) . ? C41 C42 1.32(2) . ? C42 C43 1.35(4) . ? C43 C44 1.21(8) . ? 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 N2 Ti1 N1 117.7(3) . . ? N2 Ti1 C32 106.3(4) . . ? N1 Ti1 C32 113.2(3) . . ? N2 Ti1 C25 103.8(3) . . ? N1 Ti1 C25 110.1(4) . . ? C32 Ti1 C25 104.6(4) . . ? N1 P1 C7 112.5(4) . . ? N1 P1 C8 112.1(5) . . ? C7 P1 C8 106.8(5) . . ? N1 P1 C12 109.7(5) . . ? C7 P1 C12 103.3(5) . . ? C8 P1 C12 112.1(5) . . ? N2 P2 C16 112.5(4) . . ? N2 P2 C21 109.2(4) . . ? C16 P2 C21 104.2(4) . . ? N2 P2 C17 111.5(4) . . ? C16 P2 C17 106.1(5) . . ? C21 P2 C17 113.1(5) . . ? P1 N1 Ti1 168.9(5) . . ? P2 N2 Ti1 175.2(5) . . ? C6 C1 C2 117.6(9) . . ? C6 C1 C7 119.6(8) . . ? C2 C1 C7 122.7(9) . . ? C3 C2 C1 121.9(10) . . ? C2 C3 C4 119.2(10) . . ? C5 C4 C3 120.7(10) . . ? C4 C5 C6 118.9(9) . . ? C4 C5 C16 122.0(10) . . ? C6 C5 C16 119.1(9) . . ? C5 C6 C1 121.5(9) . . ? C1 C7 P1 115.5(6) . . ? C11 C8 C10 111.5(9) . . ? C11 C8 C9 111.0(10) . . ? C10 C8 C9 106.6(9) . . ? C11 C8 P1 113.2(7) . . ? C10 C8 P1 108.3(7) . . ? C9 C8 P1 105.8(7) . . ? C15 C12 C14 109.0(10) . . ? C15 C12 C13 108.1(9) . . ? C14 C12 C13 111.2(9) . . ? C15 C12 P1 107.5(7) . . ? C14 C12 P1 113.6(8) . . ? C13 C12 P1 107.2(7) . . ? C5 C16 P2 114.5(6) . . ? C19 C17 C20 110.2(11) . . ? C19 C17 C18 109.8(10) . . ? C20 C17 C18 106.5(9) . . ? C19 C17 P2 113.7(8) . . ? C20 C17 P2 105.6(7) . . ? C18 C17 P2 110.7(8) . . ? C23 C21 C22 109.4(9) . . ? C23 C21 C24 109.2(9) . . ? C22 C21 C24 107.0(9) . . ? C23 C21 P2 114.6(8) . . ? C22 C21 P2 109.8(7) . . ? C24 C21 P2 106.5(7) . . ? C26 C25 Ti1 116.2(7) . . ? C31 C26 C27 112.3(11) . . ? C31 C26 C25 122.9(12) . . ? C27 C26 C25 124.7(12) . . ? C28 C27 C26 123.5(12) . . ? C29 C28 C27 121.7(15) . . ? C28 C29 C30 118.2(15) . . ? C29 C30 C31 120.7(13) . . ? C30 C31 C26 123.4(12) . . ? C33 C32 Ti1 122.2(6) . . ? C38 C33 C34 116.0(9) . . ? C38 C33 C32 121.5(10) . . ? C34 C33 C32 122.4(10) . . ? C35 C34 C33 121.7(10) . . ? C36 C35 C34 121.1(11) . . ? C35 C36 C37 119.2(11) . . ? C36 C37 C38 120.7(11) . . ? C33 C38 C37 121.2(10) . . ? C40 C39 C44 124(3) . . ? C41 C40 C39 119(2) . . ? C40 C41 C42 121(2) . . ? C41 C42 C43 114(3) . . ? C44 C43 C42 132(5) . . ? C43 C44 C39 110(4) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.238 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.055 #===end data_m-C6H4(CH2PCy2))2TiCl2 _database_code_CSD 215286 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C32 H52 Cl2 N2 P2 Ti' _chemical_formula_weight 645.50 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.472(14) _cell_length_b 17.37(2) _cell_length_c 17.70(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.95(2) _cell_angle_gamma 90.00 _cell_volume 3452(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.519 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.036188 _exptl_absorpt_correction_T_max 0.256597 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14456 _diffrn_reflns_av_R_equivalents 0.2252 _diffrn_reflns_av_sigmaI/netI 0.1787 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 23.55 _reflns_number_total 4995 _reflns_number_gt 2608 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1848P)^2^+31.0840P] 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_number_reflns 4995 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2322 _refine_ls_R_factor_gt 0.1585 _refine_ls_wR_factor_ref 0.4106 _refine_ls_wR_factor_gt 0.3607 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.083 _refine_ls_shift/su_mean 0.006 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 Ti1 Ti 0.3312(2) 0.76957(15) 0.21170(13) 0.0506(8) Uani 1 1 d . . . Cl1 Cl 0.2020(3) 0.6928(3) 0.1259(2) 0.0725(12) Uani 1 1 d . . . Cl2 Cl 0.3066(4) 0.8911(3) 0.1614(3) 0.0905(15) Uani 1 1 d . . . P1 P 0.5892(3) 0.6768(2) 0.2229(2) 0.0551(10) Uani 1 1 d . . . P2 P 0.2565(3) 0.7538(2) 0.3849(2) 0.0497(9) Uani 1 1 d . . . N1 N 0.4804(10) 0.7332(8) 0.2139(6) 0.063(3) Uani 1 1 d . . . N2 N 0.2931(11) 0.7694(7) 0.3045(6) 0.062(3) Uani 1 1 d . . . C1 C 0.6879(13) 0.6788(11) 0.3191(8) 0.070(4) Uani 1 1 d . . . H1A H 0.7519 0.6422 0.3195 0.084 Uiso 1 1 calc R . . H1B H 0.7234 0.7295 0.3273 0.084 Uiso 1 1 calc R . . C2 C 0.6300(12) 0.6606(9) 0.3852(8) 0.058(4) Uani 1 1 d . . . C3 C 0.6455(13) 0.5961(10) 0.4252(9) 0.065(4) Uani 1 1 d . . . H3A H 0.7000 0.5601 0.4146 0.078 Uiso 1 1 calc R . . C4 C 0.5834(17) 0.5802(10) 0.4828(10) 0.079(5) Uani 1 1 d . . . H4A H 0.5976 0.5346 0.5108 0.095 Uiso 1 1 calc R . . C5 C 0.4995(14) 0.6326(10) 0.4985(10) 0.070(4) Uani 1 1 d . . . H5A H 0.4575 0.6226 0.5370 0.083 Uiso 1 1 calc R . . C6 C 0.4800(12) 0.6990(9) 0.4564(8) 0.055(4) Uani 1 1 d . . . C7 C 0.5495(12) 0.7150(9) 0.4024(7) 0.055(4) Uani 1 1 d . . . H7A H 0.5423 0.7625 0.3775 0.066 Uiso 1 1 calc R . . C8 C 0.3857(13) 0.7563(9) 0.4671(8) 0.060(4) Uani 1 1 d . . . H8A H 0.4197 0.8076 0.4719 0.072 Uiso 1 1 calc R . . H8B H 0.3592 0.7446 0.5145 0.072 Uiso 1 1 calc R . . C9 C 0.5419(13) 0.5760(8) 0.2033(9) 0.063(4) Uani 1 1 d . . . H9A H 0.6109 0.5426 0.2214 0.076 Uiso 1 1 calc R . . C10 C 0.4971(16) 0.5621(10) 0.1171(10) 0.082(5) Uani 1 1 d . . . H10A H 0.5600 0.5745 0.0899 0.098 Uiso 1 1 calc R . . H10B H 0.4303 0.5959 0.0980 0.098 Uiso 1 1 calc R . . C11 C 0.458(2) 0.4787(14) 0.1001(14) 0.122(8) Uani 1 1 d . . . H11A H 0.5258 0.4449 0.1177 0.146 Uiso 1 1 calc R . . H11B H 0.4324 0.4718 0.0448 0.146 Uiso 1 1 calc R . . C12 C 0.3541(17) 0.4561(12) 0.1412(13) 0.100(6) Uani 1 1 d . . . H12A H 0.2834 0.4860 0.1203 0.120 Uiso 1 1 calc R . . H12B H 0.3349 0.4019 0.1332 0.120 Uiso 1 1 calc R . . C13 C 0.3967(18) 0.4729(12) 0.2280(13) 0.107(7) Uani 1 1 d . . . H13A H 0.3310 0.4640 0.2536 0.129 Uiso 1 1 calc R . . H13B H 0.4594 0.4368 0.2492 0.129 Uiso 1 1 calc R . . C14 C 0.4426(15) 0.5532(12) 0.2464(9) 0.083(5) Uani 1 1 d . . . H14A H 0.4735 0.5573 0.3015 0.100 Uiso 1 1 calc R . . H14B H 0.3770 0.5892 0.2327 0.100 Uiso 1 1 calc R . . C15 C 0.6862(12) 0.7046(8) 0.1570(8) 0.058(4) Uani 1 1 d . . . H15A H 0.6379 0.7017 0.1045 0.069 Uiso 1 1 calc R . . C16 C 0.7259(16) 0.7873(9) 0.1705(10) 0.077(5) Uani 1 1 d . . . H16A H 0.7759 0.7924 0.2216 0.092 Uiso 1 1 calc R . . H16B H 0.6569 0.8202 0.1677 0.092 Uiso 1 1 calc R . . C17 C 0.7960(16) 0.8123(10) 0.1091(11) 0.082(5) Uani 1 1 d . . . H17A H 0.7449 0.8095 0.0582 0.098 Uiso 1 1 calc R . . H17B H 0.8225 0.8651 0.1184 0.098 Uiso 1 1 calc R . . C18 C 0.9026(16) 0.7599(11) 0.1130(11) 0.087(5) Uani 1 1 d . . . H18A H 0.9466 0.7753 0.0743 0.104 Uiso 1 1 calc R . . H18B H 0.9552 0.7645 0.1633 0.104 Uiso 1 1 calc R . . C19 C 0.8627(17) 0.6781(11) 0.0996(12) 0.090(6) Uani 1 1 d . . . H19A H 0.9317 0.6451 0.1027 0.108 Uiso 1 1 calc R . . H19B H 0.8135 0.6731 0.0482 0.108 Uiso 1 1 calc R . . C20 C 0.7914(16) 0.6525(10) 0.1595(10) 0.079(5) Uani 1 1 d . . . H20A H 0.7641 0.6000 0.1489 0.095 Uiso 1 1 calc R . . H20B H 0.8421 0.6538 0.2107 0.095 Uiso 1 1 calc R . . C21 C 0.1532(12) 0.8268(8) 0.4058(8) 0.052(3) Uani 1 1 d . . . H21A H 0.1242 0.8098 0.4514 0.062 Uiso 1 1 calc R . . C22 C 0.0466(14) 0.8365(11) 0.3408(10) 0.080(5) Uani 1 1 d . . . H22A H 0.0733 0.8535 0.2950 0.096 Uiso 1 1 calc R . . H22B H 0.0077 0.7870 0.3293 0.096 Uiso 1 1 calc R . . C23 C -0.0435(18) 0.8945(12) 0.3598(12) 0.097(6) Uani 1 1 d . . . H23A H -0.0763 0.8754 0.4025 0.116 Uiso 1 1 calc R . . H23B H -0.1085 0.9006 0.3154 0.116 Uiso 1 1 calc R . . C24 C 0.0152(16) 0.9704(11) 0.3807(11) 0.089(6) Uani 1 1 d . . . H24A H -0.0414 1.0053 0.3963 0.106 Uiso 1 1 calc R . . H24B H 0.0387 0.9922 0.3356 0.106 Uiso 1 1 calc R . . C25 C 0.1243(16) 0.9633(11) 0.4458(10) 0.088(6) Uani 1 1 d . . . H25A H 0.1621 1.0132 0.4559 0.105 Uiso 1 1 calc R . . H25B H 0.0999 0.9465 0.4924 0.105 Uiso 1 1 calc R . . C26 C 0.2144(14) 0.9052(9) 0.4249(10) 0.073(4) Uani 1 1 d . . . H26A H 0.2439 0.9238 0.3807 0.087 Uiso 1 1 calc R . . H26B H 0.2816 0.8997 0.4679 0.087 Uiso 1 1 calc R . . C27 C 0.1886(16) 0.6590(8) 0.3881(9) 0.069(4) Uani 1 1 d . . . H27A H 0.2582 0.6260 0.4058 0.083 Uiso 1 1 calc R . . C28 C 0.121(2) 0.6495(11) 0.4506(11) 0.104(7) Uani 1 1 d . . . H28A H 0.1726 0.6621 0.4996 0.124 Uiso 1 1 calc R . . H28B H 0.0549 0.6856 0.4421 0.124 Uiso 1 1 calc R . . C29 C 0.073(5) 0.5691(17) 0.455(2) 0.24(2) Uani 1 1 d . . . H29A H 0.1350 0.5382 0.4864 0.290 Uiso 1 1 calc R . . H29B H 0.0074 0.5717 0.4819 0.290 Uiso 1 1 calc R . . C30 C 0.034(2) 0.5319(14) 0.3881(13) 0.118(8) Uani 1 1 d . . . H30A H -0.0471 0.5480 0.3678 0.141 Uiso 1 1 calc R . . H30B H 0.0322 0.4774 0.3995 0.141 Uiso 1 1 calc R . . C31 C 0.099(3) 0.5411(12) 0.3277(13) 0.131(10) Uani 1 1 d . . . H31A H 0.0506 0.5242 0.2792 0.158 Uiso 1 1 calc R . . H31B H 0.1702 0.5091 0.3387 0.158 Uiso 1 1 calc R . . C32 C 0.136(3) 0.6256(15) 0.3201(14) 0.181(16) Uani 1 1 d . . . H32A H 0.1911 0.6279 0.2852 0.217 Uiso 1 1 calc R . . H32B H 0.0660 0.6551 0.2972 0.217 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 Ti1 0.0286(14) 0.0623(17) 0.0605(14) 0.0037(11) 0.0085(10) 0.0060(12) Cl1 0.040(2) 0.089(3) 0.082(2) -0.011(2) -0.0012(17) 0.004(2) Cl2 0.078(3) 0.072(3) 0.115(3) 0.027(2) 0.006(3) 0.008(2) P1 0.028(2) 0.070(3) 0.067(2) -0.0016(17) 0.0088(16) 0.0047(18) P2 0.031(2) 0.056(2) 0.062(2) -0.0022(16) 0.0094(15) 0.0015(16) N1 0.033(7) 0.091(9) 0.066(7) -0.008(6) 0.010(5) 0.008(6) N2 0.046(7) 0.071(8) 0.066(7) 0.004(6) 0.009(6) 0.009(6) C1 0.027(8) 0.111(14) 0.069(9) 0.002(8) 0.003(7) 0.016(8) C2 0.033(8) 0.066(10) 0.068(8) -0.008(7) -0.003(7) 0.020(7) C3 0.035(9) 0.074(12) 0.082(10) -0.008(8) 0.004(8) 0.022(8) C4 0.072(13) 0.052(10) 0.101(12) 0.014(8) -0.007(10) 0.003(9) C5 0.033(9) 0.079(12) 0.093(11) 0.018(9) 0.005(8) -0.014(8) C6 0.023(8) 0.075(10) 0.063(8) 0.009(7) -0.001(6) 0.004(7) C7 0.043(9) 0.065(10) 0.055(7) 0.006(6) 0.008(6) 0.004(7) C8 0.044(9) 0.078(11) 0.059(8) 0.000(7) 0.016(6) 0.005(7) C9 0.036(8) 0.044(9) 0.107(11) 0.010(7) 0.008(8) -0.003(7) C10 0.068(12) 0.085(13) 0.098(12) -0.018(9) 0.029(10) -0.018(10) C11 0.107(18) 0.13(2) 0.138(18) -0.045(15) 0.055(15) -0.036(15) C12 0.057(12) 0.076(13) 0.16(2) -0.014(12) 0.011(13) -0.001(10) C13 0.056(13) 0.105(17) 0.15(2) 0.040(14) 0.004(12) -0.003(12) C14 0.049(10) 0.122(16) 0.075(10) 0.023(9) 0.005(8) -0.015(10) C15 0.034(8) 0.064(10) 0.074(9) -0.001(7) 0.009(6) -0.001(7) C16 0.060(11) 0.067(11) 0.105(12) -0.005(9) 0.022(9) 0.011(9) C17 0.056(11) 0.073(12) 0.118(13) 0.016(10) 0.021(10) -0.003(9) C18 0.060(12) 0.098(15) 0.110(13) 0.015(10) 0.036(10) -0.004(10) C19 0.063(12) 0.087(14) 0.134(15) 0.003(11) 0.051(11) 0.006(10) C20 0.076(13) 0.066(11) 0.100(12) -0.002(9) 0.029(10) -0.002(9) C21 0.031(8) 0.054(9) 0.075(8) 0.000(6) 0.024(6) 0.020(7) C22 0.042(10) 0.083(12) 0.103(12) -0.009(9) -0.013(8) 0.006(9) C23 0.070(13) 0.104(16) 0.109(14) -0.010(11) 0.002(10) 0.026(12) C24 0.072(13) 0.081(13) 0.114(13) -0.012(10) 0.020(10) 0.048(11) C25 0.074(13) 0.095(14) 0.090(12) -0.015(9) 0.007(9) 0.030(11) C26 0.043(10) 0.067(11) 0.102(12) -0.007(8) 0.001(8) 0.002(8) C27 0.083(12) 0.045(9) 0.092(11) -0.005(8) 0.044(9) -0.014(8) C28 0.14(2) 0.082(13) 0.098(13) -0.017(10) 0.056(13) -0.048(13) C29 0.43(6) 0.14(3) 0.21(3) -0.08(2) 0.20(4) -0.18(4) C30 0.12(2) 0.113(19) 0.110(16) 0.008(13) 0.007(14) -0.064(15) C31 0.21(3) 0.088(16) 0.098(14) -0.024(11) 0.036(16) -0.067(17) C32 0.31(4) 0.12(2) 0.121(19) -0.043(16) 0.08(2) -0.12(3) _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 Ti1 N2 1.785(12) . ? Ti1 N1 1.817(12) . ? Ti1 Cl2 2.287(6) . ? Ti1 Cl1 2.313(5) . ? P1 N1 1.569(13) . ? P1 C15 1.837(15) . ? P1 C9 1.845(15) . ? P1 C1 1.839(14) . ? P2 N2 1.589(12) . ? P2 C27 1.828(15) . ? P2 C21 1.825(12) . ? P2 C8 1.851(14) . ? C1 C2 1.49(2) . ? C2 C3 1.32(2) . ? C2 C7 1.40(2) . ? C3 C4 1.39(2) . ? C4 C5 1.39(2) . ? C5 C6 1.37(2) . ? C6 C7 1.394(19) . ? C6 C8 1.51(2) . ? C9 C10 1.53(2) . ? C9 C14 1.55(2) . ? C10 C11 1.53(3) . ? C11 C12 1.57(3) . ? C12 C13 1.54(3) . ? C13 C14 1.50(3) . ? C15 C20 1.50(2) . ? C15 C16 1.51(2) . ? C16 C17 1.54(2) . ? C17 C18 1.52(2) . ? C18 C19 1.50(3) . ? C19 C20 1.53(2) . ? C21 C22 1.51(2) . ? C21 C26 1.54(2) . ? C22 C23 1.53(2) . ? C23 C24 1.49(3) . ? C24 C25 1.52(2) . ? C25 C26 1.54(2) . ? C27 C32 1.36(3) . ? C27 C28 1.49(2) . ? C28 C29 1.51(3) . ? C29 C30 1.34(3) . ? C30 C31 1.43(3) . ? C31 C32 1.54(3) . ? 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 N2 Ti1 N1 112.9(5) . . ? N2 Ti1 Cl2 109.0(4) . . ? N1 Ti1 Cl2 111.7(5) . . ? N2 Ti1 Cl1 110.9(4) . . ? N1 Ti1 Cl1 106.6(4) . . ? Cl2 Ti1 Cl1 105.5(2) . . ? N1 P1 C15 110.2(7) . . ? N1 P1 C9 112.1(7) . . ? C15 P1 C9 108.9(7) . . ? N1 P1 C1 114.0(7) . . ? C15 P1 C1 104.2(7) . . ? C9 P1 C1 107.0(8) . . ? N2 P2 C27 112.0(7) . . ? N2 P2 C21 111.5(6) . . ? C27 P2 C21 108.7(7) . . ? N2 P2 C8 112.6(6) . . ? C27 P2 C8 105.9(8) . . ? C21 P2 C8 105.8(7) . . ? P1 N1 Ti1 160.9(9) . . ? P2 N2 Ti1 170.2(9) . . ? C2 C1 P1 115.7(11) . . ? C3 C2 C7 118.7(14) . . ? C3 C2 C1 124.6(14) . . ? C7 C2 C1 116.7(14) . . ? C2 C3 C4 122.1(15) . . ? C3 C4 C5 119.8(15) . . ? C6 C5 C4 119.0(16) . . ? C5 C6 C7 119.4(14) . . ? C5 C6 C8 121.9(14) . . ? C7 C6 C8 118.7(13) . . ? C6 C7 C2 120.8(14) . . ? C6 C8 P2 111.3(10) . . ? C10 C9 C14 108.8(13) . . ? C10 C9 P1 111.4(11) . . ? C14 C9 P1 111.6(12) . . ? C9 C10 C11 111.8(16) . . ? C10 C11 C12 111.3(17) . . ? C13 C12 C11 107.4(16) . . ? C14 C13 C12 114.6(16) . . ? C13 C14 C9 113.1(17) . . ? C20 C15 C16 110.8(13) . . ? C20 C15 P1 114.3(11) . . ? C16 C15 P1 110.6(10) . . ? C15 C16 C17 109.9(13) . . ? C18 C17 C16 109.4(14) . . ? C19 C18 C17 110.2(15) . . ? C18 C19 C20 110.8(15) . . ? C15 C20 C19 110.1(14) . . ? C22 C21 C26 109.3(12) . . ? C22 C21 P2 112.4(10) . . ? C26 C21 P2 111.9(10) . . ? C23 C22 C21 112.6(14) . . ? C22 C23 C24 110.2(16) . . ? C23 C24 C25 112.0(16) . . ? C26 C25 C24 111.0(13) . . ? C21 C26 C25 109.5(13) . . ? C32 C27 C28 114.1(19) . . ? C32 C27 P2 118.1(14) . . ? C28 C27 P2 114.5(11) . . ? C29 C28 C27 113.2(17) . . ? C30 C29 C28 117(2) . . ? C29 C30 C31 119(2) . . ? C30 C31 C32 111(2) . . ? C27 C32 C31 114(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 23.55 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.602 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.119 #===end