# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1185 data_fgnc/jfn-1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Zr(C5H5)2(C6H3Me2NP=CtBu)]' _chemical_formula_analytical ? _chemical_formula_sum 'C23 H28 N P Zr' _chemical_formula_weight 440.65 _chemical_melting_point ? _chemical_compound_source ? 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' 'Zr' 'Zr' -2.9673 0.5597 '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 11.622(3) _cell_length_b 21.830(8) _cell_length_c 8.389(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.01(3) _cell_angle_gamma 90.00 _cell_volume 2035.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method ? _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3811 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3563 _reflns_number_observed 2651 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+8.2446P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3561 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_obs 0.0476 _refine_ls_wR_factor_all 0.1375 _refine_ls_wR_factor_obs 0.1141 _refine_ls_goodness_of_fit_all 0.834 _refine_ls_goodness_of_fit_obs 0.817 _refine_ls_restrained_S_all 0.841 _refine_ls_restrained_S_obs 0.817 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr Zr 0.28026(4) 0.07270(2) 0.29606(6) 0.0142(2) Uani 1 d . . M1 C 0.3245 -0.0131 0.1776 0.000 Uiso 0.00 d P 1 M2 C 0.1999 0.0784 0.5106 0.000 Uiso 0.00 d P 1 P P 0.30727(12) 0.18101(6) 0.1448(2) 0.0183(3) Uani 1 d . 1 N N 0.4096(4) 0.1403(2) 0.2997(5) 0.0166(9) Uani 1 d . 1 C1 C 0.1834(5) 0.1360(2) 0.1006(6) 0.0174(11) Uani 1 d . 1 C2 C 0.0701(5) 0.1532(2) -0.0378(7) 0.0214(12) Uani 1 d . 1 C3 C -0.0393(5) 0.1552(3) 0.0282(7) 0.0265(13) Uani 1 d . 1 H3A H -0.1120(6) 0.1625(18) -0.0645(10) 0.040 Uiso 1 calc R 1 H3B H -0.0293(17) 0.1884(12) 0.1099(36) 0.040 Uiso 1 calc R 1 H3C H -0.0466(21) 0.1161(7) 0.0816(43) 0.040 Uiso 1 calc R 1 C4 C 0.0471(5) 0.1034(3) -0.1747(7) 0.0289(13) Uani 1 d . 1 H4A H -0.0219(23) 0.1153(9) -0.2685(22) 0.043 Uiso 1 calc R 1 H4B H 0.0301(35) 0.0643(5) -0.1289(15) 0.043 Uiso 1 calc R 1 H4C H 0.1185(14) 0.0991(13) -0.2133(35) 0.043 Uiso 1 calc R 1 C5 C 0.0793(6) 0.2154(3) -0.1194(9) 0.040(2) Uani 1 d . 1 H5A H 0.0041(17) 0.2237(10) -0.2071(40) 0.060 Uiso 1 calc R 1 H5B H 0.1463(27) 0.2145(7) -0.1680(50) 0.060 Uiso 1 calc R 1 H5C H 0.0932(41) 0.2478(4) -0.0349(15) 0.060 Uiso 1 calc R 1 C6 C 0.5342(5) 0.1558(2) 0.3340(6) 0.0160(11) Uani 1 d . 1 C7 C 0.5963(5) 0.1491(2) 0.2114(6) 0.0185(11) Uani 1 d . 1 C8 C 0.7194(5) 0.1605(3) 0.2581(7) 0.0264(13) Uani 1 d . 1 H8 H 0.7619(5) 0.1549(3) 0.1781(7) 0.032 Uiso 1 calc R 1 C9 C 0.7820(5) 0.1796(3) 0.4162(8) 0.0312(14) Uani 1 d . 1 H9 H 0.8664(5) 0.1862(3) 0.4453(8) 0.037 Uiso 1 calc R 1 C10 C 0.7195(5) 0.1892(3) 0.5323(7) 0.0259(13) Uani 1 d . 1 H10 H 0.7613(5) 0.2041(3) 0.6401(7) 0.031 Uiso 1 calc R 1 C11 C 0.5974(5) 0.1773(2) 0.4934(6) 0.0177(11) Uani 1 d . 1 C12 C 0.5334(5) 0.1894(3) 0.6220(7) 0.0239(12) Uani 1 d . 1 H12A H 0.5085(29) 0.1505(3) 0.6597(34) 0.036 Uiso 1 calc R 1 H12B H 0.4622(19) 0.2148(14) 0.5731(15) 0.036 Uiso 1 calc R 1 H12C H 0.5876(12) 0.2110(15) 0.7172(21) 0.036 Uiso 1 calc R 1 C13 C 0.5346(5) 0.1334(3) 0.0329(7) 0.0267(13) Uani 1 d . 1 H13A H 0.5071(31) 0.1711(3) -0.0302(12) 0.040 Uiso 1 calc R 1 H13B H 0.4652(21) 0.1070(15) 0.0267(8) 0.040 Uiso 1 calc R 1 H13C H 0.5909(12) 0.1119(16) -0.0145(15) 0.040 Uiso 1 calc R 1 C14 C 0.3233(5) 0.0148(3) 0.0555(7) 0.0273(13) Uani 1 d . 2 H14 H 0.3222(5) 0.0368(3) -0.0426(7) 0.033 Uiso 1 calc R 2 C15 C 0.4237(5) 0.0069(2) 0.1947(7) 0.0231(12) Uani 1 d . 2 H15 H 0.5023(5) 0.0226(2) 0.2085(7) 0.028 Uiso 1 calc R 2 C16 C 0.3863(5) -0.0288(2) 0.3109(7) 0.0227(12) Uani 1 d . 2 H16 H 0.4354(5) -0.0411(2) 0.4178(7) 0.027 Uiso 1 calc R 2 C17 C 0.2655(5) -0.0429(2) 0.2423(7) 0.0242(12) Uani 1 d . 2 H17 H 0.2185(5) -0.0672(2) 0.2936(7) 0.029 Uiso 1 calc R 2 C18 C 0.2240(5) -0.0153(2) 0.0848(7) 0.0262(13) Uani 1 d . 2 H18 H 0.1442(5) -0.0166(2) 0.0118(7) 0.031 Uiso 1 calc R 2 C19 C 0.2351(5) 0.1301(3) 0.5348(6) 0.0226(12) Uani 1 d . 2 H19 H 0.2636(5) 0.1710(3) 0.5544(6) 0.027 Uiso 1 calc R 2 C20 C 0.1233(5) 0.1120(3) 0.4306(7) 0.0240(12) Uani 1 d . 2 H20 H 0.0621(5) 0.1385(3) 0.3670(7) 0.029 Uiso 1 calc R 2 C21 C 0.1167(5) 0.0475(3) 0.4358(7) 0.0303(14) Uani 1 d . 2 H21 H 0.0508(5) 0.0229(3) 0.3758(7) 0.036 Uiso 1 calc R 2 C22 C 0.2254(5) 0.0260(3) 0.5459(7) 0.0275(13) Uani 1 d . 2 H22 H 0.2454(5) -0.0156(3) 0.5742(7) 0.033 Uiso 1 calc R 2 C23 C 0.2987(5) 0.0767(3) 0.6060(6) 0.0221(12) Uani 1 d . 2 H23 H 0.3775(5) 0.0756(3) 0.6816(6) 0.027 Uiso 1 calc R 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.0179(3) 0.0139(3) 0.0132(3) 0.0014(2) 0.0081(2) -0.0005(2) P 0.0186(7) 0.0178(7) 0.0190(7) 0.0038(6) 0.0063(6) -0.0021(5) N 0.018(2) 0.018(2) 0.014(2) 0.001(2) 0.005(2) -0.002(2) C1 0.022(3) 0.016(3) 0.015(3) -0.002(2) 0.008(2) -0.002(2) C2 0.019(3) 0.023(3) 0.020(3) 0.005(2) 0.002(2) -0.002(2) C3 0.021(3) 0.027(3) 0.032(3) -0.005(3) 0.008(2) 0.005(2) C4 0.024(3) 0.044(4) 0.018(3) -0.005(3) 0.005(2) -0.001(3) C5 0.027(3) 0.038(4) 0.045(4) 0.022(3) -0.005(3) -0.003(3) C6 0.021(3) 0.011(2) 0.017(3) 0.005(2) 0.008(2) 0.001(2) C7 0.023(3) 0.017(3) 0.018(3) 0.001(2) 0.010(2) 0.001(2) C8 0.024(3) 0.031(3) 0.029(3) 0.005(3) 0.016(3) 0.001(3) C9 0.015(3) 0.034(3) 0.044(4) 0.005(3) 0.007(3) 0.001(2) C10 0.026(3) 0.027(3) 0.023(3) -0.001(2) 0.004(2) -0.004(2) C11 0.023(3) 0.012(2) 0.017(3) 0.002(2) 0.005(2) 0.002(2) C12 0.030(3) 0.026(3) 0.016(3) -0.005(2) 0.009(2) -0.002(2) C13 0.035(3) 0.032(3) 0.019(3) -0.002(2) 0.017(3) -0.002(3) C14 0.044(4) 0.018(3) 0.024(3) -0.005(2) 0.016(3) 0.001(3) C15 0.028(3) 0.016(3) 0.029(3) -0.002(2) 0.013(3) 0.002(2) C16 0.032(3) 0.017(3) 0.019(3) 0.002(2) 0.007(2) 0.008(2) C17 0.028(3) 0.013(3) 0.033(3) -0.002(2) 0.012(3) -0.002(2) C18 0.033(3) 0.018(3) 0.026(3) -0.009(2) 0.006(3) 0.002(2) C19 0.027(3) 0.029(3) 0.017(3) 0.001(2) 0.013(2) 0.003(2) C20 0.024(3) 0.037(3) 0.017(3) 0.004(2) 0.016(2) 0.007(3) C21 0.029(3) 0.045(4) 0.026(3) -0.006(3) 0.021(3) -0.014(3) C22 0.041(4) 0.024(3) 0.027(3) 0.007(2) 0.024(3) 0.002(3) C23 0.028(3) 0.032(3) 0.010(2) 0.004(2) 0.010(2) 0.000(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 Zr N 2.101(4) . ? Zr C1 2.188(5) . ? Zr M1 2.2483(8) . ? Zr M2 2.2610(10) . ? Zr C16 2.520(5) . ? Zr C15 2.529(5) . ? Zr C19 2.543(5) . ? Zr C23 2.547(5) . ? Zr C14 2.551(6) . ? Zr C20 2.557(5) . ? Zr C17 2.560(5) . ? Zr C18 2.565(5) . ? Zr C21 2.568(5) . ? Zr C22 2.572(5) . ? Zr P 2.744(2) . ? P C1 1.692(5) . ? P N 1.729(4) . ? N C6 1.431(6) . ? C1 C2 1.526(7) . ? C2 C3 1.528(8) . ? C2 C5 1.538(8) . ? C2 C4 1.547(8) . ? C6 C11 1.405(7) . ? C6 C7 1.426(7) . ? C7 C8 1.391(8) . ? C7 C13 1.498(7) . ? C8 C9 1.377(8) . ? C9 C10 1.391(8) . ? C10 C11 1.384(7) . ? C11 C12 1.503(7) . ? C14 C15 1.399(8) . ? C14 C18 1.411(8) . ? C15 C16 1.412(8) . ? C16 C17 1.387(8) . ? C17 C18 1.403(8) . ? C19 C20 1.394(8) . ? C19 C23 1.414(8) . ? C20 C21 1.411(9) . ? C21 C22 1.409(8) . ? C22 C23 1.397(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 N Zr C1 77.1(2) . . ? N Zr M1 109.64(12) . . ? C1 Zr M1 109.21(14) . . ? N Zr M2 114.21(12) . . ? C1 Zr M2 108.64(14) . . ? M1 Zr M2 126.82(2) . . ? C16 Zr C15 32.5(2) . . ? C16 Zr C19 127.2(2) . . ? C15 Zr C19 148.5(2) . . ? C16 Zr C23 94.9(2) . . ? C15 Zr C23 119.7(2) . . ? C19 Zr C23 32.3(2) . . ? C16 Zr C14 53.0(2) . . ? C15 Zr C14 32.0(2) . . ? C19 Zr C14 179.4(2) . . ? C23 Zr C14 147.9(2) . . ? C16 Zr C20 132.4(2) . . ? C15 Zr C20 164.6(2) . . ? C19 Zr C20 31.7(2) . . ? C23 Zr C20 52.8(2) . . ? C14 Zr C20 147.7(2) . . ? C16 Zr C17 31.7(2) . . ? C15 Zr C17 53.0(2) . . ? C19 Zr C17 127.3(2) . . ? C23 Zr C17 101.3(2) . . ? C14 Zr C17 52.5(2) . . ? C20 Zr C17 112.9(2) . . ? C16 Zr C18 53.0(2) . . ? C15 Zr C18 53.3(2) . . ? C19 Zr C18 147.5(2) . . ? C23 Zr C18 131.3(2) . . ? C14 Zr C18 32.0(2) . . ? C20 Zr C18 119.0(2) . . ? C17 Zr C18 31.8(2) . . ? C16 Zr C21 101.9(2) . . ? C15 Zr C21 132.9(2) . . ? C19 Zr C21 52.8(2) . . ? C23 Zr C21 52.7(2) . . ? C14 Zr C21 126.7(2) . . ? C20 Zr C21 32.0(2) . . ? C17 Zr C21 81.3(2) . . ? C18 Zr C21 94.7(2) . . ? C16 Zr C22 81.1(2) . . ? C15 Zr C22 113.2(2) . . ? C19 Zr C22 52.9(2) . . ? C23 Zr C22 31.7(2) . . ? C14 Zr C22 126.9(2) . . ? C20 Zr C22 52.7(2) . . ? C17 Zr C22 74.5(2) . . ? C18 Zr C22 101.1(2) . . ? C21 Zr C22 31.8(2) . . ? N Zr P 39.03(12) . . ? C1 Zr P 38.05(13) . . ? M1 Zr P 116.18(5) . . ? M2 Zr P 116.74(4) . . ? C1 P N 102.8(2) . . ? C1 P Zr 52.9(2) . . ? N P Zr 49.95(14) . . ? C6 N P 117.6(3) . . ? C6 N Zr 147.8(3) . . ? P N Zr 91.0(2) . . ? C2 C1 P 120.9(4) . . ? C2 C1 Zr 150.0(4) . . ? P C1 Zr 89.1(2) . . ? C1 C2 C3 110.8(4) . . ? C1 C2 C5 113.5(4) . . ? C3 C2 C5 108.0(5) . . ? C1 C2 C4 108.3(4) . . ? C3 C2 C4 107.9(4) . . ? C5 C2 C4 108.1(5) . . ? C11 C6 C7 119.1(5) . . ? C11 C6 N 119.1(4) . . ? C7 C6 N 121.8(5) . . ? C8 C7 C6 118.3(5) . . ? C8 C7 C13 118.4(5) . . ? C6 C7 C13 123.2(5) . . ? C9 C8 C7 122.4(5) . . ? C8 C9 C10 118.9(5) . . ? C11 C10 C9 121.1(5) . . ? C10 C11 C6 120.1(5) . . ? C10 C11 C12 119.1(5) . . ? C6 C11 C12 120.7(5) . . ? C15 C14 C18 108.8(5) . . ? C15 C14 Zr 73.1(3) . . ? C18 C14 Zr 74.5(3) . . ? C14 C15 C16 107.1(5) . . ? C14 C15 Zr 74.9(3) . . ? C16 C15 Zr 73.4(3) . . ? C17 C16 C15 108.3(5) . . ? C17 C16 Zr 75.7(3) . . ? C15 C16 Zr 74.1(3) . . ? C16 C17 C18 108.9(5) . . ? C16 C17 Zr 72.6(3) . . ? C18 C17 Zr 74.3(3) . . ? C17 C18 C14 106.9(5) . . ? C17 C18 Zr 73.9(3) . . ? C14 C18 Zr 73.4(3) . . ? C20 C19 C23 107.9(5) . . ? C20 C19 Zr 74.7(3) . . ? C23 C19 Zr 74.0(3) . . ? C19 C20 C21 108.2(5) . . ? C19 C20 Zr 73.6(3) . . ? C21 C20 Zr 74.4(3) . . ? C22 C21 C20 107.8(5) . . ? C22 C21 Zr 74.3(3) . . ? C20 C21 Zr 73.6(3) . . ? C23 C22 C21 107.9(5) . . ? C23 C22 Zr 73.2(3) . . ? C21 C22 Zr 73.9(3) . . ? C22 C23 C19 108.2(5) . . ? C22 C23 Zr 75.2(3) . . ? C19 C23 Zr 73.7(3) . . ? _refine_diff_density_max 0.647 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.106 #=END data_fgnc/jfn-2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[TiCl2(C5H5N){P(CtBu)2PNtBu}]' _chemical_formula_analytical ? _chemical_formula_sum 'C19 H32 Cl2 N2 P2 Ti' _chemical_formula_weight 469.21 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 '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 12.728(2) _cell_length_b 12.1700(10) _cell_length_c 15.5960(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.500(10) _cell_angle_gamma 90.00 _cell_volume 2395.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method ? _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7242 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.98 _reflns_number_total 6969 _reflns_number_observed 5271 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.7779P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6968 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_all 0.0953 _refine_ls_wR_factor_obs 0.0849 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.031 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.76673(3) 0.23192(3) 0.01514(2) 0.02063(8) Uani 1 d . . Cl1 Cl 0.82850(4) 0.16464(4) 0.15152(3) 0.02936(11) Uani 1 d . . Cl2 Cl 0.70712(4) 0.08774(4) -0.07505(4) 0.03624(13) Uani 1 d . . P1 P 0.66766(4) 0.40426(4) 0.00526(3) 0.02478(11) Uani 1 d . . P2 P 0.86598(4) 0.42714(4) -0.02124(3) 0.02559(11) Uani 1 d . . N1 N 0.93873(13) 0.17827(14) -0.01601(10) 0.0259(3) Uani 1 d . . N2 N 0.63000(12) 0.27477(13) 0.03483(11) 0.0258(3) Uani 1 d . . C1 C 0.7982(2) 0.41912(15) 0.06814(12) 0.0250(4) Uani 1 d . . C2 C 0.75076(15) 0.3693(2) -0.07948(12) 0.0233(4) Uani 1 d . . C3 C 0.8284(2) 0.4657(2) 0.15827(13) 0.0321(5) Uani 1 d . . C4 C 0.7498(2) 0.4300(2) 0.21928(15) 0.0439(6) Uani 1 d . . H4A H 0.7712(2) 0.4612(2) 0.27685(15) 0.066 Uiso 1 calc R . H4B H 0.7491(2) 0.3496(2) 0.22316(15) 0.066 Uiso 1 calc R . H4C H 0.6787(2) 0.4563(2) 0.19686(15) 0.066 Uiso 1 calc R . C5 C 0.9410(2) 0.4318(2) 0.19455(14) 0.0402(5) Uani 1 d . . H5A H 0.9590(2) 0.4627(2) 0.25265(14) 0.060 Uiso 1 calc R . H5B H 0.9908(2) 0.4595(2) 0.15675(14) 0.060 Uiso 1 calc R . H5C H 0.9455(2) 0.3515(2) 0.19751(14) 0.060 Uiso 1 calc R . C6 C 0.8244(2) 0.5922(2) 0.1494(2) 0.0485(6) Uani 1 d . . H6A H 0.8434(2) 0.6258(2) 0.2064(2) 0.073 Uiso 1 calc R . H6B H 0.7525(2) 0.6149(2) 0.1257(2) 0.073 Uiso 1 calc R . H6C H 0.8745(2) 0.6160(2) 0.1105(2) 0.073 Uiso 1 calc R . C7 C 0.7211(2) 0.3753(2) -0.17752(13) 0.0317(4) Uani 1 d . . C8 C 0.8024(2) 0.3109(2) -0.22161(14) 0.0459(6) Uani 1 d . . H8A H 0.8733(2) 0.3410(2) -0.20387(14) 0.069 Uiso 1 calc R . H8B H 0.7850(2) 0.3170(2) -0.28452(14) 0.069 Uiso 1 calc R . H8C H 0.8009(2) 0.2334(2) -0.20467(14) 0.069 Uiso 1 calc R . C9 C 0.7242(2) 0.4954(2) -0.2054(2) 0.0491(7) Uani 1 d . . H9A H 0.7954(2) 0.5251(2) -0.1883(2) 0.074 Uiso 1 calc R . H9B H 0.6726(2) 0.5378(2) -0.1776(2) 0.074 Uiso 1 calc R . H9C H 0.7066(2) 0.5003(2) -0.2684(2) 0.074 Uiso 1 calc R . C10 C 0.6102(2) 0.3295(3) -0.2044(2) 0.0563(8) Uani 1 d . . H10A H 0.6079(2) 0.2524(3) -0.1865(2) 0.084 Uiso 1 calc R . H10B H 0.5927(2) 0.3346(3) -0.2673(2) 0.084 Uiso 1 calc R . H10C H 0.5588(2) 0.3721(3) -0.1765(2) 0.084 Uiso 1 calc R . C11 C 0.5225(2) 0.2422(2) 0.0509(2) 0.0399(5) Uani 1 d . . C12 C 0.4492(2) 0.2449(4) -0.0341(3) 0.104(2) Uani 1 d . . H12A H 0.4451(2) 0.3201(4) -0.0568(3) 0.156 Uiso 1 calc R . H12B H 0.3783(2) 0.2202(4) -0.0246(3) 0.156 Uiso 1 calc R . H12C H 0.4769(2) 0.1961(4) -0.0759(3) 0.156 Uiso 1 calc R . C13 C 0.4836(3) 0.3193(3) 0.1164(3) 0.0909(14) Uani 1 d . . H13A H 0.4789(3) 0.3941(3) 0.0929(3) 0.136 Uiso 1 calc R . H13B H 0.5334(3) 0.3181(3) 0.1699(3) 0.136 Uiso 1 calc R . H13C H 0.4135(3) 0.2955(3) 0.1286(3) 0.136 Uiso 1 calc R . C14 C 0.5298(2) 0.1268(2) 0.0869(2) 0.0432(6) Uani 1 d . . H14A H 0.5550(2) 0.0771(2) 0.0445(2) 0.065 Uiso 1 calc R . H14B H 0.4598(2) 0.1030(2) 0.0991(2) 0.065 Uiso 1 calc R . H14C H 0.5796(2) 0.1256(2) 0.1405(2) 0.065 Uiso 1 calc R . C15 C 1.0248(2) 0.2088(2) 0.03691(14) 0.0341(5) Uani 1 d . . H15 H 1.0155(2) 0.2513(2) 0.08646(14) 0.041 Uiso 1 calc R . C16 C 1.1264(2) 0.1819(2) 0.0233(2) 0.0441(6) Uani 1 d . . H16 H 1.1854(2) 0.2053(2) 0.0627(2) 0.053 Uiso 1 calc R . C17 C 1.1413(2) 0.1204(2) -0.0484(2) 0.0436(6) Uani 1 d . . H17 H 1.2106(2) 0.1005(2) -0.0592(2) 0.052 Uiso 1 calc R . C18 C 1.0546(2) 0.0888(2) -0.1033(2) 0.0406(5) Uani 1 d . . H18 H 1.0623(2) 0.0468(2) -0.1535(2) 0.049 Uiso 1 calc R . C19 C 0.9554(2) 0.1187(2) -0.08510(14) 0.0329(5) Uani 1 d . . H19 H 0.8955(2) 0.0956(2) -0.12373(14) 0.040 Uiso 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 Ti 0.0192(2) 0.01966(15) 0.0234(2) 0.00089(13) 0.00418(12) 0.00106(12) Cl1 0.0366(3) 0.0265(2) 0.0255(2) 0.0055(2) 0.0063(2) 0.0054(2) Cl2 0.0327(3) 0.0353(3) 0.0406(3) -0.0139(2) 0.0046(2) -0.0064(2) P1 0.0254(2) 0.0232(2) 0.0268(2) 0.0045(2) 0.0075(2) 0.0053(2) P2 0.0272(3) 0.0266(2) 0.0236(2) 0.0014(2) 0.0056(2) -0.0056(2) N1 0.0235(8) 0.0281(8) 0.0264(8) -0.0003(7) 0.0042(6) 0.0043(6) N2 0.0215(8) 0.0247(8) 0.0324(9) 0.0045(7) 0.0081(6) 0.0015(6) C1 0.0324(10) 0.0210(9) 0.0220(9) 0.0003(7) 0.0054(7) -0.0006(7) C2 0.0240(9) 0.0261(9) 0.0197(8) 0.0017(7) 0.0028(7) -0.0014(7) C3 0.0508(13) 0.0227(9) 0.0229(9) -0.0043(8) 0.0047(9) 0.0000(9) C4 0.068(2) 0.0372(12) 0.0298(11) -0.0065(9) 0.0208(11) 0.0043(11) C5 0.0544(15) 0.0377(12) 0.0263(10) -0.0082(9) -0.0031(10) -0.0057(11) C6 0.079(2) 0.0252(11) 0.0394(13) -0.0049(10) 0.0020(13) -0.0010(12) C7 0.0319(11) 0.0425(12) 0.0197(9) 0.0038(8) 0.0003(8) 0.0034(9) C8 0.059(2) 0.057(2) 0.0228(10) -0.0034(10) 0.0065(10) 0.0150(13) C9 0.060(2) 0.055(2) 0.0333(12) 0.0200(11) 0.0116(11) 0.0197(13) C10 0.0449(15) 0.088(2) 0.0307(12) 0.0047(13) -0.0138(11) -0.0076(15) C11 0.0231(10) 0.0411(12) 0.0582(15) 0.0132(11) 0.0157(10) 0.0007(9) C12 0.0254(14) 0.177(4) 0.104(3) 0.073(3) -0.013(2) -0.029(2) C13 0.086(2) 0.046(2) 0.163(4) -0.003(2) 0.100(3) 0.001(2) C14 0.0383(13) 0.0362(12) 0.058(2) 0.0029(11) 0.0176(11) -0.0114(10) C15 0.0272(10) 0.0457(13) 0.0289(10) -0.0004(9) 0.0014(8) 0.0022(9) C16 0.0252(11) 0.063(2) 0.0434(13) 0.0093(12) 0.0016(9) 0.0039(11) C17 0.0316(12) 0.0491(14) 0.0530(15) 0.0134(12) 0.0168(11) 0.0165(10) C18 0.0414(13) 0.0370(12) 0.0468(14) -0.0014(10) 0.0181(11) 0.0112(10) C19 0.0320(11) 0.0320(11) 0.0357(11) -0.0065(9) 0.0077(9) 0.0036(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 Ti N2 1.880(2) . ? Ti C2 2.221(2) . ? Ti Cl2 2.3140(6) . ? Ti Cl1 2.3187(6) . ? Ti N1 2.394(2) . ? Ti C1 2.439(2) . ? Ti P1 2.4417(6) . ? Ti P2 2.7838(6) . ? P1 N2 1.727(2) . ? P1 C1 1.825(2) . ? P1 C2 1.847(2) . ? P1 P2 2.6253(8) . ? P2 C1 1.735(2) . ? P2 C2 1.768(2) . ? N1 C15 1.336(3) . ? N1 C19 1.339(3) . ? N2 C11 1.478(3) . ? C1 C3 1.518(3) . ? C2 C7 1.528(3) . ? C3 C5 1.527(3) . ? C3 C4 1.531(3) . ? C3 C6 1.546(3) . ? C7 C10 1.523(3) . ? C7 C9 1.527(3) . ? C7 C8 1.531(3) . ? C11 C14 1.510(3) . ? C11 C13 1.516(4) . ? C11 C12 1.519(4) . ? C15 C16 1.378(3) . ? C16 C17 1.379(4) . ? C17 C18 1.361(4) . ? C18 C19 1.379(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 Ti C2 83.88(7) . . ? N2 Ti Cl2 94.16(6) . . ? C2 Ti Cl2 99.93(5) . . ? N2 Ti Cl1 99.11(5) . . ? C2 Ti Cl1 149.97(5) . . ? Cl2 Ti Cl1 109.57(2) . . ? N2 Ti N1 177.71(7) . . ? C2 Ti N1 94.43(6) . . ? Cl2 Ti N1 84.60(4) . . ? Cl1 Ti N1 83.13(4) . . ? N2 Ti C1 78.46(7) . . ? C2 Ti C1 61.25(7) . . ? Cl2 Ti C1 160.17(5) . . ? Cl1 Ti C1 89.88(5) . . ? N1 Ti C1 102.09(6) . . ? N2 Ti P1 44.82(5) . . ? C2 Ti P1 46.37(5) . . ? Cl2 Ti P1 119.17(2) . . ? Cl1 Ti P1 118.14(2) . . ? N1 Ti P1 134.41(4) . . ? C1 Ti P1 43.91(5) . . ? N2 Ti P2 104.53(5) . . ? C2 Ti P2 39.38(5) . . ? Cl2 Ti P2 130.15(2) . . ? Cl1 Ti P2 112.32(2) . . ? N1 Ti P2 74.93(4) . . ? C1 Ti P2 38.10(4) . . ? P1 Ti P2 59.89(2) . . ? N2 P1 C1 102.23(8) . . ? N2 P1 C2 100.68(8) . . ? C1 P1 C2 80.86(8) . . ? N2 P1 Ti 50.10(5) . . ? C1 P1 Ti 67.96(6) . . ? C2 P1 Ti 60.52(6) . . ? N2 P1 P2 116.41(6) . . ? C1 P1 P2 41.19(6) . . ? C2 P1 P2 42.24(6) . . ? Ti P1 P2 66.54(2) . . ? C1 P2 C2 85.65(9) . . ? C1 P2 P1 43.82(7) . . ? C2 P2 P1 44.63(6) . . ? C1 P2 Ti 60.12(6) . . ? C2 P2 Ti 52.88(6) . . ? P1 P2 Ti 53.57(2) . . ? C15 N1 C19 116.4(2) . . ? C15 N1 Ti 119.79(14) . . ? C19 N1 Ti 123.78(14) . . ? C11 N2 P1 125.87(14) . . ? C11 N2 Ti 148.31(14) . . ? P1 N2 Ti 85.09(7) . . ? C3 C1 P2 129.1(2) . . ? C3 C1 P1 129.63(15) . . ? P2 C1 P1 95.00(9) . . ? C3 C1 Ti 132.33(13) . . ? P2 C1 Ti 81.79(7) . . ? P1 C1 Ti 68.13(6) . . ? C7 C2 P2 125.13(14) . . ? C7 C2 P1 127.95(14) . . ? P2 C2 P1 93.13(9) . . ? C7 C2 Ti 133.62(14) . . ? P2 C2 Ti 87.75(8) . . ? P1 C2 Ti 73.11(6) . . ? C1 C3 C5 110.8(2) . . ? C1 C3 C4 111.2(2) . . ? C5 C3 C4 110.6(2) . . ? C1 C3 C6 106.7(2) . . ? C5 C3 C6 108.7(2) . . ? C4 C3 C6 108.7(2) . . ? C10 C7 C9 109.2(2) . . ? C10 C7 C2 110.9(2) . . ? C9 C7 C2 108.6(2) . . ? C10 C7 C8 110.2(2) . . ? C9 C7 C8 108.5(2) . . ? C2 C7 C8 109.4(2) . . ? N2 C11 C14 107.4(2) . . ? N2 C11 C13 109.8(2) . . ? C14 C11 C13 109.6(2) . . ? N2 C11 C12 108.8(2) . . ? C14 C11 C12 110.3(3) . . ? C13 C11 C12 111.0(3) . . ? N1 C15 C16 123.3(2) . . ? C15 C16 C17 119.0(2) . . ? C18 C17 C16 118.5(2) . . ? C17 C18 C19 119.0(2) . . ? N1 C19 C18 123.6(2) . . ? _refine_diff_density_max 0.373 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.067 #=END