# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Douglas W Stephan' 'Alberto Ramos' _publ_contact_author_name 'Douglas W Stephan' _publ_contact_author_email DSTEPHAN@CHEM.UTORONTO.CA _publ_section_title ; Titanium Ferrocenyl-Phosphinimide Complexes ; # Attachment 'cif.doc' data_CpFe(C5H4)PBu2(NSiMe3) _database_code_depnum_ccdc_archive 'CCDC 747506' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C21 H36 Fe N P Si' _chemical_formula_weight 417.42 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monolcinic _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 10.083(2) _cell_length_b 10.733(2) _cell_length_c 41.135(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.94(3) _cell_angle_gamma 90.00 _cell_volume 4427.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6774 _exptl_absorpt_correction_T_max 0.7475 _diffrn_ambient_temperature 150(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 20154 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9194 _reflns_number_gt 6436 _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 Rfactors 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^)+(0.0363P)^2^+2.8407P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 9194 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Fe1A Fe 0.89952(4) 0.27921(4) 0.141631(10) 0.02641(12) Uani 1 1 d . . . Fe1B Fe 1.38542(4) -0.49495(4) 0.106964(10) 0.02765(12) Uani 1 1 d . . . P1B P 1.30146(8) -0.21992(7) 0.055806(18) 0.02476(18) Uani 1 1 d . . . P1A P 0.86580(8) 0.00641(7) 0.188861(18) 0.02493(18) Uani 1 1 d . . . N1B N 1.1497(2) -0.2295(2) 0.04770(6) 0.0305(6) Uani 1 1 d . . . N1A N 0.9703(3) 0.0519(2) 0.21601(6) 0.0331(6) Uani 1 1 d . . . Si1B Si 0.98779(8) -0.24311(8) 0.03599(2) 0.0278(2) Uani 1 1 d . . . Si1A Si 1.09944(9) 0.06551(8) 0.24424(2) 0.0338(2) Uani 1 1 d . . . C1A C 0.8745(3) 0.0930(3) 0.15107(7) 0.0252(7) Uani 1 1 d . . . C1B C 1.3592(3) -0.3115(3) 0.09189(7) 0.0245(7) Uani 1 1 d . . . C2A C 1.0006(3) 0.1165(3) 0.13866(7) 0.0271(7) Uani 1 1 d . . . H2AA H 1.0904 0.0973 0.1503 0.033 Uiso 1 1 calc R . . C2B C 1.4894(3) -0.3299(3) 0.10944(8) 0.0304(7) Uani 1 1 d . . . H2BA H 1.5768 -0.3148 0.1006 0.036 Uiso 1 1 calc R . . C3B C 1.4719(3) -0.3734(3) 0.14135(8) 0.0340(8) Uani 1 1 d . . . H3BA H 1.5448 -0.3939 0.1589 0.041 Uiso 1 1 calc R . . C3A C 0.9761(3) 0.1704(3) 0.10703(7) 0.0321(7) Uani 1 1 d . . . H3AA H 1.0454 0.1963 0.0927 0.038 Uiso 1 1 calc R . . C4A C 0.8368(3) 0.1829(3) 0.09965(7) 0.0325(8) Uani 1 1 d . . . H4AA H 0.7906 0.2198 0.0792 0.039 Uiso 1 1 calc R . . C4B C 1.3324(3) -0.3829(3) 0.14395(8) 0.0344(8) Uani 1 1 d . . . H4BA H 1.2907 -0.4115 0.1637 0.041 Uiso 1 1 calc R . . C5B C 1.2633(3) -0.3461(3) 0.11387(7) 0.0295(7) Uani 1 1 d . . . H5BA H 1.1642 -0.3446 0.1087 0.035 Uiso 1 1 calc R . . C5A C 0.7732(3) 0.1355(3) 0.12636(7) 0.0277(7) Uani 1 1 d . . . H5AA H 0.6749 0.1334 0.1279 0.033 Uiso 1 1 calc R . . C6A C 0.9093(3) 0.3751(3) 0.18510(8) 0.0357(8) Uani 1 1 d . . . H6AA H 0.9061 0.3377 0.2073 0.043 Uiso 1 1 calc R . . C6B C 1.4047(4) -0.6167(3) 0.06939(9) 0.0449(9) Uani 1 1 d . . . H6BA H 1.4195 -0.5942 0.0465 0.054 Uiso 1 1 calc R . . C7B C 1.5050(4) -0.6398(3) 0.09555(11) 0.0500(10) Uani 1 1 d . . . H7BA H 1.6034 -0.6354 0.0943 0.060 Uiso 1 1 calc R . . C7A C 1.0258(3) 0.3963(3) 0.16932(8) 0.0354(8) Uani 1 1 d . . . H7AA H 1.1192 0.3766 0.1785 0.043 Uiso 1 1 calc R . . C8A C 0.9868(4) 0.4503(3) 0.13809(8) 0.0367(8) Uani 1 1 d . . . H8AA H 1.0477 0.4757 0.1216 0.044 Uiso 1 1 calc R . . C8B C 1.4424(4) -0.6690(3) 0.12342(9) 0.0464(10) Uani 1 1 d . . . H8BA H 1.4884 -0.6893 0.1455 0.056 Uiso 1 1 calc R . . C9B C 1.3046(4) -0.6657(3) 0.11496(8) 0.0384(8) Uani 1 1 d . . . H9BA H 1.2353 -0.6829 0.1301 0.046 Uiso 1 1 calc R . . C9A C 0.8453(4) 0.4618(3) 0.13483(9) 0.0391(9) Uani 1 1 d . . . H9AA H 0.7892 0.4964 0.1155 0.047 Uiso 1 1 calc R . . C10B C 1.2792(4) -0.6329(3) 0.08174(8) 0.0382(8) Uani 1 1 d . . . H10A H 1.1895 -0.6241 0.0691 0.046 Uiso 1 1 calc R . . C10A C 0.7978(4) 0.4155(3) 0.16373(8) 0.0367(8) Uani 1 1 d . . . H10B H 0.7023 0.4115 0.1683 0.044 Uiso 1 1 calc R . . C11A C 0.6939(3) 0.0241(3) 0.20179(7) 0.0297(7) Uani 1 1 d . . . C11B C 1.3929(3) -0.2718(3) 0.02089(7) 0.0306(7) Uani 1 1 d . . . C12A C 0.5819(3) -0.0385(3) 0.17930(8) 0.0386(8) Uani 1 1 d . . . H12A H 0.4962 -0.0240 0.1879 0.058 Uiso 1 1 calc R . . H12B H 0.5988 -0.1283 0.1784 0.058 Uiso 1 1 calc R . . H12C H 0.5794 -0.0031 0.1573 0.058 Uiso 1 1 calc R . . C12B C 1.5377(3) -0.3100(3) 0.03129(8) 0.0373(8) Uani 1 1 d . . . H12D H 1.5802 -0.3357 0.0120 0.056 Uiso 1 1 calc R . . H12E H 1.5390 -0.3795 0.0468 0.056 Uiso 1 1 calc R . . H12F H 1.5863 -0.2391 0.0418 0.056 Uiso 1 1 calc R . . C13A C 0.6934(4) -0.0268(3) 0.23670(7) 0.0385(8) Uani 1 1 d . . . H13A H 0.6039 -0.0180 0.2437 0.058 Uiso 1 1 calc R . . H13B H 0.7574 0.0201 0.2515 0.058 Uiso 1 1 calc R . . H13C H 0.7186 -0.1151 0.2371 0.058 Uiso 1 1 calc R . . C13B C 1.3149(3) -0.3845(3) 0.00580(8) 0.0382(8) Uani 1 1 d . . . H13D H 1.3582 -0.4156 -0.0129 0.057 Uiso 1 1 calc R . . H13E H 1.2233 -0.3592 -0.0016 0.057 Uiso 1 1 calc R . . H13F H 1.3135 -0.4505 0.0222 0.057 Uiso 1 1 calc R . . C14A C 0.6635(3) 0.1641(3) 0.20363(8) 0.0353(8) Uani 1 1 d . . . H14A H 0.5738 0.1757 0.2103 0.053 Uiso 1 1 calc R . . H14B H 0.6685 0.2021 0.1821 0.053 Uiso 1 1 calc R . . H14C H 0.7289 0.2037 0.2197 0.053 Uiso 1 1 calc R . . C14B C 1.3894(4) -0.1711(3) -0.00564(8) 0.0412(9) Uani 1 1 d . . . H14D H 1.4377 -0.2007 -0.0236 0.062 Uiso 1 1 calc R . . H14E H 1.4317 -0.0950 0.0036 0.062 Uiso 1 1 calc R . . H14F H 1.2966 -0.1533 -0.0139 0.062 Uiso 1 1 calc R . . C15B C 1.3498(3) -0.0584(3) 0.06986(7) 0.0292(7) Uani 1 1 d . . . C15A C 0.8946(3) -0.1578(3) 0.17524(7) 0.0310(7) Uani 1 1 d . . . C16A C 1.0445(3) -0.1728(3) 0.17270(9) 0.0426(9) Uani 1 1 d . . . H16A H 1.0627 -0.2578 0.1657 0.064 Uiso 1 1 calc R . . H16B H 1.0939 -0.1568 0.1941 0.064 Uiso 1 1 calc R . . H16C H 1.0726 -0.1133 0.1567 0.064 Uiso 1 1 calc R . . C16B C 1.2957(4) -0.0400(3) 0.10332(8) 0.0371(8) Uani 1 1 d . . . H16D H 1.3191 0.0435 0.1116 0.056 Uiso 1 1 calc R . . H16E H 1.3351 -0.1026 0.1188 0.056 Uiso 1 1 calc R . . H16F H 1.1985 -0.0494 0.1008 0.056 Uiso 1 1 calc R . . C17B C 1.2783(3) 0.0371(3) 0.04609(8) 0.0364(8) Uani 1 1 d . . . H17A H 1.3035 0.1216 0.0533 0.055 Uiso 1 1 calc R . . H17B H 1.1816 0.0269 0.0458 0.055 Uiso 1 1 calc R . . H17C H 1.3045 0.0235 0.0241 0.055 Uiso 1 1 calc R . . C17A C 0.8194(4) -0.1872(3) 0.14149(8) 0.0393(8) Uani 1 1 d . . . H17D H 0.8374 -0.2734 0.1355 0.059 Uiso 1 1 calc R . . H17E H 0.8496 -0.1305 0.1251 0.059 Uiso 1 1 calc R . . H17F H 0.7234 -0.1762 0.1425 0.059 Uiso 1 1 calc R . . C18B C 1.5007(3) -0.0327(3) 0.07390(8) 0.0346(8) Uani 1 1 d . . . H18A H 1.5168 0.0533 0.0813 0.052 Uiso 1 1 calc R . . H18B H 1.5366 -0.0447 0.0529 0.052 Uiso 1 1 calc R . . H18C H 1.5447 -0.0902 0.0901 0.052 Uiso 1 1 calc R . . C18A C 0.8552(4) -0.2525(3) 0.20064(8) 0.0415(9) Uani 1 1 d . . . H18D H 0.8714 -0.3371 0.1931 0.062 Uiso 1 1 calc R . . H18E H 0.7605 -0.2427 0.2035 0.062 Uiso 1 1 calc R . . H18F H 0.9087 -0.2378 0.2216 0.062 Uiso 1 1 calc R . . C19B C 0.9117(3) -0.3685(3) 0.05976(9) 0.0430(9) Uani 1 1 d . . . H19A H 0.9576 -0.4476 0.0568 0.064 Uiso 1 1 calc R . . H19B H 0.8170 -0.3772 0.0519 0.064 Uiso 1 1 calc R . . H19C H 0.9207 -0.3464 0.0830 0.064 Uiso 1 1 calc R . . C19A C 1.2623(4) 0.0705(4) 0.22627(13) 0.0739(14) Uani 1 1 d . . . H19D H 1.2616 0.1396 0.2107 0.111 Uiso 1 1 calc R . . H19E H 1.2757 -0.0081 0.2150 0.111 Uiso 1 1 calc R . . H19F H 1.3348 0.0827 0.2438 0.111 Uiso 1 1 calc R . . C20B C 0.8970(3) -0.0944(3) 0.04246(8) 0.0387(8) Uani 1 1 d . . . H20A H 0.9139 -0.0692 0.0654 0.058 Uiso 1 1 calc R . . H20B H 0.8010 -0.1071 0.0369 0.058 Uiso 1 1 calc R . . H20C H 0.9284 -0.0291 0.0285 0.058 Uiso 1 1 calc R . . C20A C 1.1048(4) -0.0673(3) 0.27413(9) 0.0624(13) Uani 1 1 d . . . H20D H 1.0210 -0.0702 0.2842 0.094 Uiso 1 1 calc R . . H20E H 1.1793 -0.0552 0.2911 0.094 Uiso 1 1 calc R . . H20F H 1.1169 -0.1458 0.2626 0.094 Uiso 1 1 calc R . . C21B C 0.9510(4) -0.2850(3) -0.00816(8) 0.0440(9) Uani 1 1 d . . . H21A H 0.9969 -0.3628 -0.0125 0.066 Uiso 1 1 calc R . . H21B H 0.9822 -0.2182 -0.0217 0.066 Uiso 1 1 calc R . . H21C H 0.8547 -0.2960 -0.0134 0.066 Uiso 1 1 calc R . . C21A C 1.0859(4) 0.2132(3) 0.26756(8) 0.0470(10) Uani 1 1 d . . . H21D H 1.0023 0.2132 0.2778 0.070 Uiso 1 1 calc R . . H21E H 1.0868 0.2843 0.2526 0.070 Uiso 1 1 calc R . . H21F H 1.1614 0.2197 0.2845 0.070 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 Fe1A 0.0292(3) 0.0229(2) 0.0274(2) -0.00073(18) 0.00369(18) -0.00154(19) Fe1B 0.0277(3) 0.0231(2) 0.0314(2) -0.00095(19) -0.00041(18) 0.00154(19) P1B 0.0236(4) 0.0247(4) 0.0256(4) -0.0015(3) 0.0011(3) -0.0003(3) P1A 0.0279(4) 0.0231(4) 0.0238(4) -0.0003(3) 0.0029(3) -0.0002(3) N1B 0.0222(14) 0.0346(15) 0.0338(14) -0.0025(12) -0.0016(11) 0.0005(12) N1A 0.0360(16) 0.0320(15) 0.0301(14) -0.0006(12) -0.0017(12) -0.0001(12) Si1B 0.0234(5) 0.0301(5) 0.0291(4) -0.0006(4) -0.0012(3) 0.0010(4) Si1A 0.0300(5) 0.0307(5) 0.0390(5) -0.0050(4) -0.0048(4) 0.0025(4) C1A 0.0314(18) 0.0172(15) 0.0271(15) -0.0028(12) 0.0041(13) -0.0006(13) C1B 0.0255(17) 0.0189(15) 0.0286(15) -0.0035(12) 0.0001(13) 0.0015(12) C2A 0.0241(17) 0.0252(17) 0.0327(16) -0.0019(13) 0.0064(13) 0.0020(13) C2B 0.0277(18) 0.0245(17) 0.0374(18) -0.0019(14) -0.0043(14) -0.0003(13) C3B 0.044(2) 0.0240(17) 0.0313(17) -0.0043(14) -0.0074(15) 0.0021(15) C3A 0.038(2) 0.0275(17) 0.0322(17) -0.0029(13) 0.0121(14) -0.0016(14) C4A 0.041(2) 0.0289(18) 0.0270(16) -0.0010(13) 0.0009(14) -0.0045(15) C4B 0.047(2) 0.0272(18) 0.0294(16) 0.0000(14) 0.0047(15) 0.0019(15) C5B 0.0330(19) 0.0241(17) 0.0320(17) -0.0029(13) 0.0053(14) 0.0023(14) C5A 0.0295(18) 0.0247(16) 0.0286(16) -0.0018(13) 0.0017(13) -0.0018(13) C6A 0.044(2) 0.0298(18) 0.0336(17) -0.0071(14) 0.0072(15) -0.0038(16) C6B 0.073(3) 0.0232(18) 0.041(2) -0.0049(15) 0.0181(19) 0.0012(18) C7B 0.031(2) 0.0279(19) 0.092(3) -0.014(2) 0.008(2) 0.0045(16) C7A 0.035(2) 0.0303(18) 0.0400(18) -0.0081(15) -0.0010(15) -0.0048(15) C8A 0.045(2) 0.0206(17) 0.0450(19) -0.0035(15) 0.0087(16) -0.0076(15) C8B 0.056(3) 0.0269(19) 0.052(2) -0.0006(17) -0.014(2) 0.0080(17) C9B 0.047(2) 0.0244(18) 0.045(2) -0.0030(15) 0.0093(17) -0.0031(16) C9A 0.045(2) 0.0205(17) 0.051(2) 0.0033(15) -0.0008(17) -0.0015(15) C10B 0.038(2) 0.0281(18) 0.046(2) -0.0108(15) -0.0072(16) 0.0003(15) C10A 0.038(2) 0.0224(17) 0.051(2) -0.0072(15) 0.0108(16) -0.0027(15) C11A 0.0294(18) 0.0311(18) 0.0294(16) 0.0016(13) 0.0071(13) -0.0021(14) C11B 0.0284(18) 0.0320(18) 0.0319(16) -0.0018(14) 0.0049(13) 0.0013(14) C12A 0.031(2) 0.045(2) 0.0409(19) 0.0001(16) 0.0061(15) -0.0068(16) C12B 0.0302(19) 0.040(2) 0.0426(19) -0.0045(16) 0.0097(15) 0.0025(15) C13A 0.047(2) 0.037(2) 0.0334(18) 0.0037(15) 0.0117(16) -0.0023(16) C13B 0.039(2) 0.037(2) 0.0393(19) -0.0098(15) 0.0071(16) 0.0016(16) C14A 0.035(2) 0.0357(19) 0.0367(18) 0.0016(15) 0.0105(15) 0.0063(15) C14B 0.049(2) 0.042(2) 0.0336(18) -0.0029(15) 0.0117(16) -0.0013(17) C15B 0.0321(19) 0.0248(16) 0.0301(16) 0.0002(13) 0.0001(14) -0.0003(14) C15A 0.038(2) 0.0242(17) 0.0313(17) -0.0020(13) 0.0068(14) 0.0017(14) C16A 0.045(2) 0.0307(19) 0.053(2) -0.0035(16) 0.0087(18) 0.0107(16) C16B 0.049(2) 0.0267(18) 0.0358(18) -0.0043(14) 0.0061(16) 0.0012(16) C17B 0.040(2) 0.0280(18) 0.0402(19) 0.0021(14) -0.0015(15) 0.0024(15) C17A 0.055(2) 0.0288(19) 0.0337(18) -0.0058(14) 0.0044(16) -0.0030(16) C18B 0.0322(19) 0.0289(18) 0.0411(18) -0.0022(14) -0.0036(15) -0.0078(14) C18A 0.058(2) 0.0272(19) 0.0404(19) 0.0058(15) 0.0089(17) 0.0028(16) C19B 0.032(2) 0.043(2) 0.053(2) 0.0081(18) 0.0027(17) -0.0026(16) C19A 0.035(2) 0.060(3) 0.129(4) -0.023(3) 0.018(3) -0.003(2) C20B 0.031(2) 0.039(2) 0.045(2) -0.0018(16) -0.0002(15) 0.0044(15) C20A 0.087(3) 0.038(2) 0.054(2) 0.0014(19) -0.028(2) 0.012(2) C21B 0.042(2) 0.051(2) 0.0372(18) -0.0054(17) -0.0067(16) 0.0061(18) C21A 0.056(3) 0.039(2) 0.042(2) -0.0069(17) -0.0124(18) 0.0031(18) _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 Fe1A C2A 2.032(3) . ? Fe1A C9A 2.046(3) . ? Fe1A C8A 2.048(3) . ? Fe1A C7A 2.049(3) . ? Fe1A C10A 2.052(3) . ? Fe1A C3A 2.053(3) . ? Fe1A C4A 2.055(3) . ? Fe1A C5A 2.056(3) . ? Fe1A C1A 2.057(3) . ? Fe1A C6A 2.057(3) . ? Fe1B C9B 2.046(3) . ? Fe1B C10B 2.046(3) . ? Fe1B C6B 2.049(3) . ? Fe1B C8B 2.049(3) . ? Fe1B C3B 2.051(3) . ? Fe1B C7B 2.051(3) . ? Fe1B C4B 2.053(3) . ? Fe1B C5B 2.055(3) . ? Fe1B C2B 2.055(3) . ? Fe1B C1B 2.073(3) . ? P1B N1B 1.535(3) . ? P1B C1B 1.825(3) . ? P1B C11B 1.870(3) . ? P1B C15B 1.876(3) . ? P1A N1A 1.533(3) . ? P1A C1A 1.821(3) . ? P1A C11A 1.874(3) . ? P1A C15A 1.881(3) . ? N1B Si1B 1.660(3) . ? N1A Si1A 1.659(3) . ? Si1B C21B 1.871(3) . ? Si1B C20B 1.873(3) . ? Si1B C19B 1.874(3) . ? Si1A C21A 1.865(3) . ? Si1A C19A 1.870(4) . ? Si1A C20A 1.880(4) . ? C1A C5A 1.438(4) . ? C1A C2A 1.440(4) . ? C1B C5B 1.440(4) . ? C1B C2B 1.445(4) . ? C2A C3A 1.422(4) . ? C2B C3B 1.421(4) . ? C3B C4B 1.425(5) . ? C3A C4A 1.412(4) . ? C4A C5A 1.422(4) . ? C4B C5B 1.412(4) . ? C6A C7A 1.418(5) . ? C6A C10A 1.422(5) . ? C6B C7B 1.420(5) . ? C6B C10B 1.422(5) . ? C7B C8B 1.400(5) . ? C7A C8A 1.427(4) . ? C8A C9A 1.424(5) . ? C8B C9B 1.397(5) . ? C9B C10B 1.409(5) . ? C9A C10A 1.417(5) . ? C11A C13A 1.537(4) . ? C11A C14A 1.537(4) . ? C11A C12A 1.538(4) . ? C11B C14B 1.534(4) . ? C11B C12B 1.534(4) . ? C11B C13B 1.538(4) . ? C15B C18B 1.538(4) . ? C15B C17B 1.543(4) . ? C15B C16B 1.545(4) . ? C15A C16A 1.535(5) . ? C15A C18A 1.538(4) . ? C15A C17A 1.544(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 C2A Fe1A C9A 160.66(13) . . ? C2A Fe1A C8A 122.99(13) . . ? C9A Fe1A C8A 40.72(13) . . ? C2A Fe1A C7A 105.91(13) . . ? C9A Fe1A C7A 68.30(13) . . ? C8A Fe1A C7A 40.77(12) . . ? C2A Fe1A C10A 156.35(13) . . ? C9A Fe1A C10A 40.46(13) . . ? C8A Fe1A C10A 68.32(13) . . ? C7A Fe1A C10A 68.08(13) . . ? C2A Fe1A C3A 40.75(12) . . ? C9A Fe1A C3A 124.36(14) . . ? C8A Fe1A C3A 105.40(13) . . ? C7A Fe1A C3A 118.55(14) . . ? C10A Fe1A C3A 162.52(13) . . ? C2A Fe1A C4A 68.28(12) . . ? C9A Fe1A C4A 108.19(13) . . ? C8A Fe1A C4A 119.22(13) . . ? C7A Fe1A C4A 153.53(13) . . ? C10A Fe1A C4A 127.31(14) . . ? C3A Fe1A C4A 40.22(12) . . ? C2A Fe1A C5A 68.62(12) . . ? C9A Fe1A C5A 121.90(13) . . ? C8A Fe1A C5A 155.19(12) . . ? C7A Fe1A C5A 163.61(12) . . ? C10A Fe1A C5A 110.35(13) . . ? C3A Fe1A C5A 68.09(13) . . ? C4A Fe1A C5A 40.46(12) . . ? C2A Fe1A C1A 41.25(12) . . ? C9A Fe1A C1A 156.99(13) . . ? C8A Fe1A C1A 161.24(13) . . ? C7A Fe1A C1A 124.93(12) . . ? C10A Fe1A C1A 122.16(13) . . ? C3A Fe1A C1A 68.92(12) . . ? C4A Fe1A C1A 68.70(12) . . ? C5A Fe1A C1A 40.94(11) . . ? C2A Fe1A C6A 120.21(13) . . ? C9A Fe1A C6A 68.14(14) . . ? C8A Fe1A C6A 68.34(13) . . ? C7A Fe1A C6A 40.40(13) . . ? C10A Fe1A C6A 40.48(13) . . ? C3A Fe1A C6A 154.16(14) . . ? C4A Fe1A C6A 164.80(14) . . ? C5A Fe1A C6A 127.84(13) . . ? C1A Fe1A C6A 108.54(12) . . ? C9B Fe1B C10B 40.27(13) . . ? C9B Fe1B C6B 67.68(14) . . ? C10B Fe1B C6B 40.63(14) . . ? C9B Fe1B C8B 39.91(14) . . ? C10B Fe1B C8B 67.78(14) . . ? C6B Fe1B C8B 67.81(14) . . ? C9B Fe1B C3B 127.35(13) . . ? C10B Fe1B C3B 166.61(14) . . ? C6B Fe1B C3B 149.23(15) . . ? C8B Fe1B C3B 105.49(13) . . ? C9B Fe1B C7B 67.13(15) . . ? C10B Fe1B C7B 67.95(14) . . ? C6B Fe1B C7B 40.54(15) . . ? C8B Fe1B C7B 39.94(15) . . ? C3B Fe1B C7B 114.93(14) . . ? C9B Fe1B C4B 105.49(14) . . ? C10B Fe1B C4B 129.58(14) . . ? C6B Fe1B C4B 170.09(15) . . ? C8B Fe1B C4B 112.01(14) . . ? C3B Fe1B C4B 40.64(13) . . ? C7B Fe1B C4B 144.85(15) . . ? C9B Fe1B C5B 114.82(14) . . ? C10B Fe1B C5B 110.07(13) . . ? C6B Fe1B C5B 134.86(14) . . ? C8B Fe1B C5B 144.56(15) . . ? C3B Fe1B C5B 68.19(13) . . ? C7B Fe1B C5B 174.72(15) . . ? C4B Fe1B C5B 40.22(12) . . ? C9B Fe1B C2B 166.78(13) . . ? C10B Fe1B C2B 152.42(13) . . ? C6B Fe1B C2B 119.97(14) . . ? C8B Fe1B C2B 130.18(14) . . ? C3B Fe1B C2B 40.50(12) . . ? C7B Fe1B C2B 110.82(14) . . ? C4B Fe1B C2B 68.22(13) . . ? C5B Fe1B C2B 68.47(13) . . ? C9B Fe1B C1B 149.13(13) . . ? C10B Fe1B C1B 119.47(12) . . ? C6B Fe1B C1B 113.55(13) . . ? C8B Fe1B C1B 170.96(14) . . ? C3B Fe1B C1B 68.55(11) . . ? C7B Fe1B C1B 135.33(15) . . ? C4B Fe1B C1B 68.31(12) . . ? C5B Fe1B C1B 40.82(12) . . ? C2B Fe1B C1B 40.96(11) . . ? N1B P1B C1B 111.55(14) . . ? N1B P1B C11B 111.88(14) . . ? C1B P1B C11B 108.87(14) . . ? N1B P1B C15B 110.51(14) . . ? C1B P1B C15B 101.31(13) . . ? C11B P1B C15B 112.26(14) . . ? N1A P1A C1A 111.66(14) . . ? N1A P1A C11A 110.29(14) . . ? C1A P1A C11A 108.56(14) . . ? N1A P1A C15A 113.56(14) . . ? C1A P1A C15A 101.62(13) . . ? C11A P1A C15A 110.78(14) . . ? P1B N1B Si1B 175.52(19) . . ? P1A N1A Si1A 165.47(19) . . ? N1B Si1B C21B 113.13(15) . . ? N1B Si1B C20B 111.38(14) . . ? C21B Si1B C20B 106.99(15) . . ? N1B Si1B C19B 110.80(14) . . ? C21B Si1B C19B 106.45(17) . . ? C20B Si1B C19B 107.80(16) . . ? N1A Si1A C21A 109.93(15) . . ? N1A Si1A C19A 112.56(19) . . ? C21A Si1A C19A 107.04(19) . . ? N1A Si1A C20A 110.99(16) . . ? C21A Si1A C20A 107.87(17) . . ? C19A Si1A C20A 108.3(2) . . ? C5A C1A C2A 106.4(3) . . ? C5A C1A P1A 132.2(2) . . ? C2A C1A P1A 120.9(2) . . ? C5A C1A Fe1A 69.52(16) . . ? C2A C1A Fe1A 68.46(16) . . ? P1A C1A Fe1A 132.44(15) . . ? C5B C1B C2B 106.6(3) . . ? C5B C1B P1B 118.1(2) . . ? C2B C1B P1B 132.6(2) . . ? C5B C1B Fe1B 68.90(16) . . ? C2B C1B Fe1B 68.86(16) . . ? P1B C1B Fe1B 140.80(15) . . ? C3A C2A C1A 108.6(3) . . ? C3A C2A Fe1A 70.40(17) . . ? C1A C2A Fe1A 70.29(16) . . ? C3B C2B C1B 108.3(3) . . ? C3B C2B Fe1B 69.58(17) . . ? C1B C2B Fe1B 70.17(16) . . ? C2B C3B C4B 108.1(3) . . ? C2B C3B Fe1B 69.92(17) . . ? C4B C3B Fe1B 69.76(17) . . ? C4A C3A C2A 108.1(3) . . ? C4A C3A Fe1A 69.99(18) . . ? C2A C3A Fe1A 68.85(17) . . ? C3A C4A C5A 108.5(3) . . ? C3A C4A Fe1A 69.79(17) . . ? C5A C4A Fe1A 69.81(17) . . ? C5B C4B C3B 108.4(3) . . ? C5B C4B Fe1B 69.95(18) . . ? C3B C4B Fe1B 69.60(18) . . ? C4B C5B C1B 108.6(3) . . ? C4B C5B Fe1B 69.83(18) . . ? C1B C5B Fe1B 70.28(17) . . ? C4A C5A C1A 108.4(3) . . ? C4A C5A Fe1A 69.73(17) . . ? C1A C5A Fe1A 69.54(16) . . ? C7A C6A C10A 107.9(3) . . ? C7A C6A Fe1A 69.49(18) . . ? C10A C6A Fe1A 69.59(18) . . ? C7B C6B C10B 107.4(3) . . ? C7B C6B Fe1B 69.8(2) . . ? C10B C6B Fe1B 69.59(19) . . ? C8B C7B C6B 108.3(3) . . ? C8B C7B Fe1B 69.9(2) . . ? C6B C7B Fe1B 69.63(19) . . ? C6A C7A C8A 108.3(3) . . ? C6A C7A Fe1A 70.10(18) . . ? C8A C7A Fe1A 69.58(18) . . ? C9A C8A C7A 107.4(3) . . ? C9A C8A Fe1A 69.55(18) . . ? C7A C8A Fe1A 69.65(18) . . ? C9B C8B C7B 108.1(3) . . ? C9B C8B Fe1B 69.93(19) . . ? C7B C8B Fe1B 70.1(2) . . ? C8B C9B C10B 108.9(3) . . ? C8B C9B Fe1B 70.2(2) . . ? C10B C9B Fe1B 69.87(19) . . ? C10A C9A C8A 108.3(3) . . ? C10A C9A Fe1A 70.03(18) . . ? C8A C9A Fe1A 69.73(18) . . ? C9B C10B C6B 107.3(3) . . ? C9B C10B Fe1B 69.86(18) . . ? C6B C10B Fe1B 69.78(19) . . ? C9A C10A C6A 108.1(3) . . ? C9A C10A Fe1A 69.52(19) . . ? C6A C10A Fe1A 69.93(18) . . ? C13A C11A C14A 106.3(3) . . ? C13A C11A C12A 109.5(3) . . ? C14A C11A C12A 108.6(3) . . ? C13A C11A P1A 108.8(2) . . ? C14A C11A P1A 107.9(2) . . ? C12A C11A P1A 115.3(2) . . ? C14B C11B C12B 109.7(3) . . ? C14B C11B C13B 107.1(3) . . ? C12B C11B C13B 109.5(3) . . ? C14B C11B P1B 111.1(2) . . ? C12B C11B P1B 113.3(2) . . ? C13B C11B P1B 105.8(2) . . ? C18B C15B C17B 109.9(3) . . ? C18B C15B C16B 108.5(3) . . ? C17B C15B C16B 107.1(3) . . ? C18B C15B P1B 115.0(2) . . ? C17B C15B P1B 109.2(2) . . ? C16B C15B P1B 106.7(2) . . ? C16A C15A C18A 107.6(3) . . ? C16A C15A C17A 108.2(3) . . ? C18A C15A C17A 109.8(3) . . ? C16A C15A P1A 107.6(2) . . ? C18A C15A P1A 111.0(2) . . ? C17A C15A P1A 112.5(2) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.426 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.083 #===end data_[TiCp*Cl2(NPtBu2Fc)] _database_code_depnum_ccdc_archive 'CCDC 747507' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H42 Cl2 Fe N P Ti' _chemical_formula_weight 598.25 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' Fe Fe 0.3463 0.8444 '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 9.1534(4) _cell_length_b 15.9165(7) _cell_length_c 19.9410(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2905.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.78 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6330 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 296(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 26143 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6667 _reflns_number_gt 5618 _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 Rfactors 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^)+(0.0370P)^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 constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(15) _refine_ls_number_reflns 6667 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Fe1 Fe 0.00416(4) 0.93852(2) 0.016865(18) 0.01966(9) Uani 1 1 d . . . Ti1 Ti -0.16345(5) 0.90629(3) 0.30096(2) 0.01860(12) Uani 1 1 d . . . Cl1 Cl -0.11619(9) 1.02936(5) 0.35891(4) 0.0377(2) Uani 1 1 d . . . Cl2 Cl -0.39838(8) 0.87381(6) 0.33556(4) 0.0363(2) Uani 1 1 d . . . P1 P -0.26273(7) 0.97932(4) 0.15035(3) 0.01734(15) Uani 1 1 d . . . N1 N -0.1923(2) 0.94130(15) 0.21738(10) 0.0189(5) Uani 1 1 d . . . C1 C -0.1054(3) 0.76014(17) 0.30512(14) 0.0246(6) Uani 1 1 d . . . C2 C -0.0877(3) 0.78912(18) 0.37249(14) 0.0236(6) Uani 1 1 d . . . C3 C 0.0260(3) 0.84797(18) 0.37367(13) 0.0229(6) Uani 1 1 d . . . C4 C 0.0777(3) 0.85857(18) 0.30659(14) 0.0238(6) Uani 1 1 d . . . C5 C 0.0004(4) 0.80190(17) 0.26511(13) 0.0243(6) Uani 1 1 d . . . C6 C -0.2047(4) 0.6926(2) 0.28333(16) 0.0366(8) Uani 1 1 d . . . H6A H -0.1581 0.6392 0.2896 0.055 Uiso 1 1 calc R . . H6B H -0.2281 0.7001 0.2368 0.055 Uiso 1 1 calc R . . H6C H -0.2928 0.6947 0.3094 0.055 Uiso 1 1 calc R . . C7 C -0.1731(4) 0.7597(2) 0.43189(14) 0.0318(7) Uani 1 1 d . . . H7A H -0.1239 0.7131 0.4524 0.048 Uiso 1 1 calc R . . H7B H -0.2688 0.7425 0.4177 0.048 Uiso 1 1 calc R . . H7C H -0.1816 0.8047 0.4637 0.048 Uiso 1 1 calc R . . C8 C 0.0906(4) 0.8891(2) 0.43440(14) 0.0338(8) Uani 1 1 d . . . H8A H 0.1630 0.8527 0.4537 0.051 Uiso 1 1 calc R . . H8B H 0.0150 0.8995 0.4667 0.051 Uiso 1 1 calc R . . H8C H 0.1353 0.9413 0.4217 0.051 Uiso 1 1 calc R . . C9 C 0.2004(3) 0.9157(2) 0.28675(16) 0.0381(9) Uani 1 1 d . . . H9A H 0.2917 0.8868 0.2919 0.057 Uiso 1 1 calc R . . H9B H 0.1995 0.9647 0.3148 0.057 Uiso 1 1 calc R . . H9C H 0.1884 0.9323 0.2408 0.057 Uiso 1 1 calc R . . C10 C 0.0341(4) 0.7843(2) 0.19300(14) 0.0352(8) Uani 1 1 d . . . H10A H 0.1031 0.7390 0.1901 0.053 Uiso 1 1 calc R . . H10B H 0.0748 0.8336 0.1726 0.053 Uiso 1 1 calc R . . H10C H -0.0541 0.7689 0.1700 0.053 Uiso 1 1 calc R . . C11 C -0.4038(3) 0.90630(19) 0.11703(13) 0.0227(6) Uani 1 1 d . . . C12 C -0.4317(3) 0.9198(2) 0.04203(13) 0.0287(7) Uani 1 1 d . . . H12A H -0.5052 0.8812 0.0269 0.043 Uiso 1 1 calc R . . H12B H -0.3429 0.9104 0.0175 0.043 Uiso 1 1 calc R . . H12C H -0.4645 0.9764 0.0347 0.043 Uiso 1 1 calc R . . C13 C -0.3444(4) 0.81761(18) 0.12859(16) 0.0314(7) Uani 1 1 d . . . H13A H -0.4134 0.7772 0.1121 0.047 Uiso 1 1 calc R . . H13B H -0.3292 0.8088 0.1757 0.047 Uiso 1 1 calc R . . H13C H -0.2534 0.8112 0.1052 0.047 Uiso 1 1 calc R . . C14 C -0.5460(3) 0.9144(2) 0.15613(15) 0.0343(8) Uani 1 1 d . . . H14A H -0.6172 0.8764 0.1379 0.051 Uiso 1 1 calc R . . H14B H -0.5816 0.9709 0.1527 0.051 Uiso 1 1 calc R . . H14C H -0.5288 0.9009 0.2024 0.051 Uiso 1 1 calc R . . C15 C -0.3340(3) 1.08640(17) 0.16994(13) 0.0232(6) Uani 1 1 d . . . C16 C -0.1995(3) 1.14179(19) 0.18277(16) 0.0311(7) Uani 1 1 d . . . H16A H -0.2305 1.1980 0.1930 0.047 Uiso 1 1 calc R . . H16B H -0.1390 1.1425 0.1434 0.047 Uiso 1 1 calc R . . H16C H -0.1449 1.1195 0.2198 0.047 Uiso 1 1 calc R . . C17 C -0.4229(4) 1.1247(2) 0.11223(14) 0.0322(8) Uani 1 1 d . . . H17A H -0.4562 1.1796 0.1248 0.048 Uiso 1 1 calc R . . H17B H -0.5055 1.0895 0.1028 0.048 Uiso 1 1 calc R . . H17C H -0.3625 1.1288 0.0730 0.048 Uiso 1 1 calc R . . C18 C -0.4252(3) 1.0853(2) 0.23495(14) 0.0297(7) Uani 1 1 d . . . H18A H -0.4605 1.1409 0.2442 0.045 Uiso 1 1 calc R . . H18B H -0.3654 1.0665 0.2715 0.045 Uiso 1 1 calc R . . H18C H -0.5065 1.0478 0.2296 0.045 Uiso 1 1 calc R . . C21 C -0.1236(3) 0.99815(17) 0.08781(13) 0.0187(6) Uani 1 1 d . . . C22 C 0.0282(3) 1.00119(16) 0.10617(13) 0.0209(6) Uani 1 1 d . . . H22A H 0.0708 0.9779 0.1473 0.025 Uiso 1 1 calc R . . C23 C 0.1056(3) 1.04244(17) 0.05488(14) 0.0242(6) Uani 1 1 d . . . H23A H 0.2110 1.0531 0.0544 0.029 Uiso 1 1 calc R . . C24 C 0.0056(3) 1.06517(17) 0.00376(13) 0.0266(6) Uani 1 1 d . . . H24A H 0.0295 1.0949 -0.0379 0.032 Uiso 1 1 calc R . . C25 C -0.1346(3) 1.03822(16) 0.02369(13) 0.0219(6) Uani 1 1 d . . . H25A H -0.2247 1.0455 -0.0022 0.026 Uiso 1 1 calc R . . C26 C -0.0324(4) 0.81241(19) 0.00551(16) 0.0363(8) Uani 1 1 d . . . H26A H -0.0955 0.7775 0.0338 0.044 Uiso 1 1 calc R . . C27 C 0.1172(4) 0.8277(2) 0.01579(15) 0.0358(8) Uani 1 1 d . . . H27A H 0.1769 0.8052 0.0524 0.043 Uiso 1 1 calc R . . C28 C 0.1659(4) 0.8805(2) -0.03583(16) 0.0344(8) Uani 1 1 d . . . H28A H 0.2658 0.9013 -0.0416 0.041 Uiso 1 1 calc R . . C29 C 0.0467(4) 0.8983(2) -0.07797(15) 0.0373(9) Uani 1 1 d . . . H29A H 0.0490 0.9333 -0.1184 0.045 Uiso 1 1 calc R . . C30 C -0.0754(4) 0.8558(2) -0.05249(17) 0.0397(9) Uani 1 1 d . . . H30A H -0.1739 0.8564 -0.0718 0.048 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 Fe1 0.01961(19) 0.02317(19) 0.01620(18) -0.00195(16) 0.00019(18) 0.00197(19) Ti1 0.0172(2) 0.0251(3) 0.0136(2) -0.0006(2) 0.0006(2) 0.0032(2) Cl1 0.0517(5) 0.0338(4) 0.0275(4) -0.0112(3) -0.0100(4) 0.0100(4) Cl2 0.0203(4) 0.0572(5) 0.0315(4) 0.0110(4) 0.0067(3) 0.0056(4) P1 0.0161(3) 0.0215(4) 0.0145(3) -0.0011(3) -0.0007(3) 0.0008(3) N1 0.0184(12) 0.0234(12) 0.0149(10) -0.0008(9) -0.0032(9) -0.0005(10) C1 0.0284(16) 0.0223(15) 0.0231(14) -0.0032(13) 0.0003(14) 0.0082(12) C2 0.0254(16) 0.0245(15) 0.0208(13) 0.0044(13) 0.0000(12) 0.0066(13) C3 0.0208(16) 0.0286(15) 0.0193(13) 0.0012(12) -0.0024(12) 0.0036(12) C4 0.0184(15) 0.0299(16) 0.0229(14) 0.0037(13) -0.0001(13) 0.0066(12) C5 0.0242(14) 0.0300(16) 0.0187(13) -0.0021(12) 0.0003(14) 0.0109(15) C6 0.042(2) 0.0309(18) 0.0366(19) -0.0039(14) -0.0035(15) -0.0056(15) C7 0.0390(18) 0.0314(17) 0.0251(15) 0.0071(13) 0.0014(15) 0.0042(15) C8 0.0333(18) 0.047(2) 0.0215(15) -0.0008(14) -0.0074(14) 0.0002(16) C9 0.0193(16) 0.058(2) 0.0372(18) 0.0063(17) 0.0037(13) -0.0006(15) C10 0.039(2) 0.046(2) 0.0204(14) -0.0017(15) 0.0019(14) 0.0171(15) C11 0.0203(14) 0.0292(15) 0.0185(13) -0.0030(12) -0.0029(12) -0.0041(13) C12 0.0274(16) 0.0346(19) 0.0240(14) -0.0012(13) -0.0061(13) -0.0057(13) C13 0.0342(18) 0.0279(16) 0.0321(16) -0.0040(13) -0.0055(15) -0.0070(14) C14 0.0224(15) 0.048(2) 0.0321(16) -0.0033(15) -0.0001(14) -0.0078(14) C15 0.0253(15) 0.0230(15) 0.0214(13) -0.0018(12) -0.0036(12) 0.0049(13) C16 0.0361(19) 0.0209(15) 0.0364(17) -0.0063(13) -0.0025(15) 0.0005(13) C17 0.0353(19) 0.0334(18) 0.0279(16) -0.0023(14) -0.0011(14) 0.0136(15) C18 0.0299(17) 0.0348(19) 0.0244(14) -0.0027(14) 0.0016(13) 0.0106(14) C21 0.0211(14) 0.0186(14) 0.0162(12) -0.0021(11) 0.0019(11) 0.0016(11) C22 0.0239(15) 0.0207(14) 0.0181(13) -0.0037(11) -0.0020(11) 0.0022(12) C23 0.0253(15) 0.0218(16) 0.0256(14) -0.0024(12) 0.0008(13) -0.0055(12) C24 0.0349(16) 0.0223(13) 0.0227(13) 0.0032(12) 0.0078(14) -0.0013(15) C25 0.0267(15) 0.0213(14) 0.0177(13) 0.0004(12) -0.0027(12) 0.0060(11) C26 0.043(2) 0.0242(16) 0.0417(19) -0.0123(14) 0.0204(16) -0.0008(14) C27 0.049(2) 0.0355(18) 0.0227(15) -0.0085(15) -0.0060(16) 0.0201(16) C28 0.0270(16) 0.0390(19) 0.0372(17) -0.0075(15) 0.0106(15) 0.0048(15) C29 0.058(2) 0.0356(19) 0.0184(14) -0.0053(14) 0.0034(15) 0.0179(17) C30 0.0272(19) 0.044(2) 0.048(2) -0.0299(18) -0.0103(17) 0.0098(16) _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 Fe1 C24 2.033(3) . ? Fe1 C29 2.034(3) . ? Fe1 C28 2.037(3) . ? Fe1 C25 2.037(3) . ? Fe1 C23 2.043(3) . ? Fe1 C30 2.044(3) . ? Fe1 C27 2.045(3) . ? Fe1 C26 2.047(3) . ? Fe1 C22 2.053(3) . ? Fe1 C21 2.066(3) . ? Ti1 N1 1.777(2) . ? Ti1 Cl1 2.3151(9) . ? Ti1 Cl2 2.3169(9) . ? Ti1 C4 2.337(3) . ? Ti1 C5 2.350(3) . ? Ti1 C1 2.388(3) . ? Ti1 C3 2.444(3) . ? Ti1 C2 2.448(3) . ? P1 N1 1.603(2) . ? P1 C21 1.808(3) . ? P1 C11 1.860(3) . ? P1 C15 1.866(3) . ? C1 C5 1.420(4) . ? C1 C2 1.430(4) . ? C1 C6 1.473(4) . ? C2 C3 1.400(4) . ? C2 C7 1.494(4) . ? C3 C4 1.429(4) . ? C3 C8 1.498(4) . ? C4 C5 1.414(4) . ? C4 C9 1.498(4) . ? C5 C10 1.497(4) . ? C11 C14 1.523(4) . ? C11 C13 1.530(4) . ? C11 C12 1.532(4) . ? C15 C17 1.535(4) . ? C15 C16 1.536(4) . ? C15 C18 1.542(4) . ? C21 C25 1.432(4) . ? C21 C22 1.438(4) . ? C22 C23 1.407(4) . ? C23 C24 1.417(4) . ? C24 C25 1.410(4) . ? C26 C30 1.403(5) . ? C26 C27 1.406(5) . ? C27 C28 1.401(5) . ? C28 C29 1.406(5) . ? C29 C30 1.402(5) . ? 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 C24 Fe1 C29 101.03(12) . . ? C24 Fe1 C28 112.27(12) . . ? C29 Fe1 C28 40.40(13) . . ? C24 Fe1 C25 40.54(11) . . ? C29 Fe1 C25 115.26(12) . . ? C28 Fe1 C25 147.24(12) . . ? C24 Fe1 C23 40.69(11) . . ? C29 Fe1 C23 120.85(13) . . ? C28 Fe1 C23 103.22(13) . . ? C25 Fe1 C23 68.14(11) . . ? C24 Fe1 C30 123.65(13) . . ? C29 Fe1 C30 40.21(13) . . ? C28 Fe1 C30 67.52(13) . . ? C25 Fe1 C30 108.96(12) . . ? C23 Fe1 C30 159.19(14) . . ? C24 Fe1 C27 148.29(14) . . ? C29 Fe1 C27 67.78(12) . . ? C28 Fe1 C27 40.15(13) . . ? C25 Fe1 C27 171.13(13) . . ? C23 Fe1 C27 118.19(13) . . ? C30 Fe1 C27 67.52(13) . . ? C24 Fe1 C26 163.54(13) . . ? C29 Fe1 C26 67.66(13) . . ? C28 Fe1 C26 67.48(13) . . ? C25 Fe1 C26 132.00(12) . . ? C23 Fe1 C26 155.40(13) . . ? C30 Fe1 C26 40.12(13) . . ? C27 Fe1 C26 40.18(13) . . ? C24 Fe1 C22 68.22(10) . . ? C29 Fe1 C22 159.85(13) . . ? C28 Fe1 C22 126.16(13) . . ? C25 Fe1 C22 68.31(11) . . ? C23 Fe1 C22 40.17(11) . . ? C30 Fe1 C22 159.76(13) . . ? C27 Fe1 C22 111.96(12) . . ? C26 Fe1 C22 126.15(12) . . ? C24 Fe1 C21 68.66(11) . . ? C29 Fe1 C21 152.80(12) . . ? C28 Fe1 C21 166.61(12) . . ? C25 Fe1 C21 40.85(10) . . ? C23 Fe1 C21 68.35(11) . . ? C30 Fe1 C21 123.89(12) . . ? C27 Fe1 C21 133.61(12) . . ? C26 Fe1 C21 115.69(11) . . ? C22 Fe1 C21 40.85(11) . . ? N1 Ti1 Cl1 103.34(8) . . ? N1 Ti1 Cl2 102.21(7) . . ? Cl1 Ti1 Cl2 102.33(4) . . ? N1 Ti1 C4 106.69(10) . . ? Cl1 Ti1 C4 94.27(8) . . ? Cl2 Ti1 C4 142.17(8) . . ? N1 Ti1 C5 91.79(10) . . ? Cl1 Ti1 C5 129.12(8) . . ? Cl2 Ti1 C5 121.69(8) . . ? C4 Ti1 C5 35.11(10) . . ? N1 Ti1 C1 111.79(10) . . ? Cl1 Ti1 C1 139.95(8) . . ? Cl2 Ti1 C1 88.78(8) . . ? C4 Ti1 C1 58.10(10) . . ? C5 Ti1 C1 34.88(10) . . ? N1 Ti1 C3 141.36(10) . . ? Cl1 Ti1 C3 83.83(7) . . ? Cl2 Ti1 C3 113.40(7) . . ? C4 Ti1 C3 34.69(9) . . ? C5 Ti1 C3 57.25(9) . . ? C1 Ti1 C3 56.73(10) . . ? N1 Ti1 C2 145.83(10) . . ? Cl1 Ti1 C2 107.50(7) . . ? Cl2 Ti1 C2 85.38(7) . . ? C4 Ti1 C2 57.11(10) . . ? C5 Ti1 C2 57.17(9) . . ? C1 Ti1 C2 34.36(9) . . ? C3 Ti1 C2 33.27(9) . . ? N1 P1 C21 110.77(12) . . ? N1 P1 C11 109.96(12) . . ? C21 P1 C11 110.25(12) . . ? N1 P1 C15 108.12(12) . . ? C21 P1 C15 103.83(13) . . ? C11 P1 C15 113.76(13) . . ? P1 N1 Ti1 163.81(15) . . ? C5 C1 C2 107.4(3) . . ? C5 C1 C6 126.6(3) . . ? C2 C1 C6 125.6(3) . . ? C5 C1 Ti1 71.10(16) . . ? C2 C1 Ti1 75.14(15) . . ? C6 C1 Ti1 124.3(2) . . ? C3 C2 C1 108.4(2) . . ? C3 C2 C7 125.8(3) . . ? C1 C2 C7 125.8(3) . . ? C3 C2 Ti1 73.18(16) . . ? C1 C2 Ti1 70.50(15) . . ? C7 C2 Ti1 123.50(19) . . ? C2 C3 C4 108.0(2) . . ? C2 C3 C8 126.8(3) . . ? C4 C3 C8 125.0(3) . . ? C2 C3 Ti1 73.55(16) . . ? C4 C3 Ti1 68.58(15) . . ? C8 C3 Ti1 126.4(2) . . ? C5 C4 C3 107.9(3) . . ? C5 C4 C9 127.4(3) . . ? C3 C4 C9 124.5(3) . . ? C5 C4 Ti1 72.93(17) . . ? C3 C4 Ti1 76.73(16) . . ? C9 C4 Ti1 119.8(2) . . ? C4 C5 C1 108.1(2) . . ? C4 C5 C10 125.3(3) . . ? C1 C5 C10 126.3(3) . . ? C4 C5 Ti1 71.96(16) . . ? C1 C5 Ti1 74.02(16) . . ? C10 C5 Ti1 123.79(19) . . ? C14 C11 C13 107.7(2) . . ? C14 C11 C12 110.2(2) . . ? C13 C11 C12 109.6(2) . . ? C14 C11 P1 110.96(19) . . ? C13 C11 P1 106.02(19) . . ? C12 C11 P1 112.1(2) . . ? C17 C15 C16 108.8(2) . . ? C17 C15 C18 110.3(2) . . ? C16 C15 C18 107.5(2) . . ? C17 C15 P1 112.99(19) . . ? C16 C15 P1 106.21(19) . . ? C18 C15 P1 110.76(19) . . ? C25 C21 C22 106.3(2) . . ? C25 C21 P1 129.8(2) . . ? C22 C21 P1 120.72(19) . . ? C25 C21 Fe1 68.48(15) . . ? C22 C21 Fe1 69.07(15) . . ? P1 C21 Fe1 142.65(15) . . ? C23 C22 C21 108.5(2) . . ? C23 C22 Fe1 69.52(15) . . ? C21 C22 Fe1 70.07(14) . . ? C22 C23 C24 108.5(2) . . ? C22 C23 Fe1 70.31(15) . . ? C24 C23 Fe1 69.28(16) . . ? C25 C24 C23 107.9(2) . . ? C25 C24 Fe1 69.90(16) . . ? C23 C24 Fe1 70.03(15) . . ? C24 C25 C21 108.8(2) . . ? C24 C25 Fe1 69.56(16) . . ? C21 C25 Fe1 70.67(15) . . ? C30 C26 C27 108.0(3) . . ? C30 C26 Fe1 69.80(18) . . ? C27 C26 Fe1 69.82(18) . . ? C28 C27 C26 107.8(3) . . ? C28 C27 Fe1 69.61(18) . . ? C26 C27 Fe1 70.00(18) . . ? C27 C28 C29 108.3(3) . . ? C27 C28 Fe1 70.24(17) . . ? C29 C28 Fe1 69.70(18) . . ? C30 C29 C28 107.7(3) . . ? C30 C29 Fe1 70.26(17) . . ? C28 C29 Fe1 69.90(17) . . ? C29 C30 C26 108.2(3) . . ? C29 C30 Fe1 69.53(18) . . ? C26 C30 Fe1 70.08(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.322 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.062 #===end data_[TiCp*Me2(NPtBu2Fc)] _database_code_depnum_ccdc_archive 'CCDC 747508' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H48 Fe N P Ti' _chemical_formula_weight 557.41 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' Fe Fe 0.3463 0.8444 '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 8.4917(17) _cell_length_b 15.639(3) _cell_length_c 22.514(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.91(3) _cell_angle_gamma 90.00 _cell_volume 2974.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.880 _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 18221 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6727 _reflns_number_gt 4803 _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 Rfactors 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^)+(0.0643P)^2^+2.5235P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 6727 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Fe1 Fe 0.40115(5) 0.13153(3) 0.125245(18) 0.02176(13) Uani 1 1 d . . . Ti1 Ti 0.48462(6) 0.22860(3) 0.35504(2) 0.02038(14) Uani 1 1 d . . . P1 P 0.53153(9) 0.31319(4) 0.21985(3) 0.02028(17) Uani 1 1 d . . . N1 N 0.5152(3) 0.28409(15) 0.28629(10) 0.0216(5) Uani 1 1 d . . . C25 C 0.2842(3) 0.19638(18) 0.18631(13) 0.0237(6) Uani 1 1 d . . . H25A H 0.2762 0.1784 0.2276 0.028 Uiso 1 1 calc R . . C21 C 0.4058(3) 0.24941(18) 0.16684(12) 0.0216(6) Uani 1 1 d . . . C15 C 0.4463(4) 0.42319(18) 0.20762(14) 0.0291(7) Uani 1 1 d . . . C14 C 0.8019(4) 0.2192(2) 0.22950(15) 0.0321(7) Uani 1 1 d . . . H14A H 0.9102 0.2113 0.2220 0.048 Uiso 1 1 calc R . . H14B H 0.7388 0.1732 0.2117 0.048 Uiso 1 1 calc R . . H14C H 0.7950 0.2198 0.2718 0.048 Uiso 1 1 calc R . . C29 C 0.5209(4) 0.0686(2) 0.06375(14) 0.0316(7) Uani 1 1 d . . . H29A H 0.5437 0.0909 0.0249 0.038 Uiso 1 1 calc R . . C28 C 0.6185(4) 0.0768(2) 0.11793(15) 0.0345(8) Uani 1 1 d . . . H28A H 0.7208 0.1063 0.1233 0.041 Uiso 1 1 calc R . . C22 C 0.3720(4) 0.25775(19) 0.10310(13) 0.0284(7) Uani 1 1 d . . . H22A H 0.4352 0.2900 0.0767 0.034 Uiso 1 1 calc R . . C1 C 0.5158(4) 0.19182(19) 0.46259(13) 0.0308(7) Uani 1 1 d . . . C30 C 0.3842(4) 0.02219(19) 0.07536(15) 0.0336(8) Uani 1 1 d . . . H30A H 0.2960 0.0064 0.0459 0.040 Uiso 1 1 calc R . . C4 C 0.5663(3) 0.32793(19) 0.43217(13) 0.0244(6) Uani 1 1 d . . . C5 C 0.4538(3) 0.27578(18) 0.45661(12) 0.0239(6) Uani 1 1 d . . . C11 C 0.7405(4) 0.30451(19) 0.20238(14) 0.0280(7) Uani 1 1 d . . . C24 C 0.1778(4) 0.1734(2) 0.13621(14) 0.0316(7) Uani 1 1 d . . . H24A H 0.0834 0.1375 0.1369 0.038 Uiso 1 1 calc R . . C20 C 0.5354(4) 0.10011(19) 0.33076(14) 0.0340(8) Uani 1 1 d . . . H20A H 0.5313 0.0959 0.2881 0.051 Uiso 1 1 calc R . . H20B H 0.4584 0.0622 0.3449 0.051 Uiso 1 1 calc R . . H20C H 0.6391 0.0845 0.3484 0.051 Uiso 1 1 calc R . . C18 C 0.2670(4) 0.4129(2) 0.20998(16) 0.0395(8) Uani 1 1 d . . . H18A H 0.2163 0.4676 0.2041 0.059 Uiso 1 1 calc R . . H18B H 0.2473 0.3904 0.2482 0.059 Uiso 1 1 calc R . . H18C H 0.2253 0.3743 0.1791 0.059 Uiso 1 1 calc R . . C13 C 0.8404(4) 0.3767(2) 0.23295(17) 0.0416(9) Uani 1 1 d . . . H13A H 0.9477 0.3715 0.2236 0.062 Uiso 1 1 calc R . . H13B H 0.8378 0.3729 0.2754 0.062 Uiso 1 1 calc R . . H13C H 0.7981 0.4309 0.2191 0.062 Uiso 1 1 calc R . . C2 C 0.6671(4) 0.1931(2) 0.44186(14) 0.0363(8) Uani 1 1 d . . . C8 C 0.8518(4) 0.3086(3) 0.40309(17) 0.0565(12) Uani 1 1 d . . . H8A H 0.9216 0.3255 0.4373 0.085 Uiso 1 1 calc R . . H8B H 0.8314 0.3567 0.3770 0.085 Uiso 1 1 calc R . . H8C H 0.9004 0.2638 0.3822 0.085 Uiso 1 1 calc R . . C27 C 0.5433(4) 0.0363(2) 0.16318(16) 0.0394(8) Uani 1 1 d . . . H27A H 0.5844 0.0323 0.2054 0.047 Uiso 1 1 calc R . . C26 C 0.3983(4) 0.0022(2) 0.13697(16) 0.0395(9) Uani 1 1 d . . . H26A H 0.3215 -0.0300 0.1578 0.047 Uiso 1 1 calc R . . C10 C 0.3032(4) 0.3067(2) 0.47883(15) 0.0368(8) Uani 1 1 d . . . H10A H 0.3228 0.3215 0.5203 0.055 Uiso 1 1 calc R . . H10B H 0.2249 0.2623 0.4740 0.055 Uiso 1 1 calc R . . H10C H 0.2655 0.3561 0.4564 0.055 Uiso 1 1 calc R . . C3 C 0.6994(4) 0.2770(2) 0.42288(14) 0.0327(8) Uani 1 1 d . . . C9 C 0.5516(5) 0.4235(2) 0.42389(15) 0.0399(8) Uani 1 1 d . . . H9A H 0.5909 0.4518 0.4603 0.060 Uiso 1 1 calc R . . H9B H 0.4424 0.4383 0.4138 0.060 Uiso 1 1 calc R . . H9C H 0.6121 0.4412 0.3923 0.060 Uiso 1 1 calc R . . C17 C 0.4770(5) 0.4647(2) 0.14825(16) 0.0449(9) Uani 1 1 d . . . H17A H 0.4300 0.5206 0.1456 0.067 Uiso 1 1 calc R . . H17B H 0.4312 0.4300 0.1158 0.067 Uiso 1 1 calc R . . H17C H 0.5890 0.4695 0.1462 0.067 Uiso 1 1 calc R . . C23 C 0.2320(4) 0.2113(2) 0.08492(14) 0.0341(8) Uani 1 1 d . . . H23A H 0.1817 0.2061 0.0439 0.041 Uiso 1 1 calc R . . C16 C 0.5081(5) 0.4820(2) 0.25926(16) 0.0404(8) Uani 1 1 d . . . H16A H 0.4640 0.5381 0.2526 0.061 Uiso 1 1 calc R . . H16B H 0.6215 0.4852 0.2614 0.061 Uiso 1 1 calc R . . H16C H 0.4776 0.4595 0.2961 0.061 Uiso 1 1 calc R . . C19 C 0.2308(4) 0.2192(2) 0.35038(14) 0.0376(8) Uani 1 1 d . . . H19A H 0.1856 0.2313 0.3104 0.056 Uiso 1 1 calc R . . H19B H 0.1917 0.2596 0.3774 0.056 Uiso 1 1 calc R . . H19C H 0.2017 0.1624 0.3612 0.056 Uiso 1 1 calc R . . C7 C 0.7840(6) 0.1196(3) 0.44592(19) 0.0699(15) Uani 1 1 d . . . H7A H 0.8413 0.1188 0.4850 0.105 Uiso 1 1 calc R . . H7B H 0.8567 0.1268 0.4164 0.105 Uiso 1 1 calc R . . H7C H 0.7279 0.0667 0.4390 0.105 Uiso 1 1 calc R . . C12 C 0.7583(4) 0.3050(2) 0.13521(15) 0.0390(8) Uani 1 1 d . . . H12A H 0.8684 0.3006 0.1292 0.058 Uiso 1 1 calc R . . H12B H 0.7160 0.3573 0.1179 0.058 Uiso 1 1 calc R . . H12C H 0.7018 0.2574 0.1165 0.058 Uiso 1 1 calc R . . C6 C 0.4370(6) 0.1163(2) 0.48744(17) 0.0562(12) Uani 1 1 d . . . H6A H 0.4646 0.1136 0.5298 0.084 Uiso 1 1 calc R . . H6B H 0.4714 0.0650 0.4693 0.084 Uiso 1 1 calc R . . H6C H 0.3242 0.1217 0.4792 0.084 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 Fe1 0.0253(2) 0.0230(2) 0.0170(2) -0.00194(16) 0.00187(17) 0.00099(17) Ti1 0.0204(3) 0.0244(3) 0.0165(3) -0.00202(19) 0.0026(2) 0.0001(2) P1 0.0222(4) 0.0198(4) 0.0192(4) -0.0009(3) 0.0039(3) -0.0004(3) N1 0.0206(12) 0.0269(13) 0.0171(12) -0.0028(10) 0.0018(10) -0.0017(10) C25 0.0203(15) 0.0290(15) 0.0221(15) -0.0054(12) 0.0039(12) 0.0018(12) C21 0.0262(15) 0.0214(14) 0.0167(14) -0.0009(11) 0.0005(11) 0.0048(12) C15 0.0403(19) 0.0212(15) 0.0257(16) 0.0015(12) 0.0031(14) 0.0028(13) C14 0.0229(16) 0.0409(19) 0.0330(18) -0.0058(14) 0.0054(13) 0.0051(14) C29 0.0425(19) 0.0285(16) 0.0259(16) -0.0069(13) 0.0134(14) 0.0017(14) C28 0.0313(18) 0.0302(17) 0.042(2) -0.0146(15) 0.0044(15) 0.0055(14) C22 0.0366(18) 0.0279(16) 0.0203(15) 0.0023(12) 0.0008(13) 0.0063(14) C1 0.051(2) 0.0244(15) 0.0164(15) -0.0012(12) 0.0017(14) 0.0044(15) C30 0.0397(19) 0.0258(16) 0.0353(18) -0.0138(13) 0.0035(15) -0.0029(14) C4 0.0251(15) 0.0287(15) 0.0193(14) -0.0034(12) 0.0022(12) -0.0011(13) C5 0.0263(16) 0.0297(16) 0.0156(14) -0.0020(11) 0.0019(12) 0.0021(13) C11 0.0225(15) 0.0320(16) 0.0302(17) -0.0026(13) 0.0067(13) -0.0024(13) C24 0.0233(16) 0.0392(18) 0.0308(17) -0.0095(14) -0.0048(13) 0.0033(14) C20 0.052(2) 0.0252(15) 0.0244(17) -0.0031(13) 0.0028(15) -0.0012(15) C18 0.038(2) 0.0340(18) 0.047(2) -0.0022(15) 0.0056(16) 0.0166(16) C13 0.0315(19) 0.047(2) 0.047(2) -0.0052(17) 0.0067(16) -0.0137(16) C2 0.042(2) 0.045(2) 0.0198(16) -0.0107(14) -0.0097(14) 0.0199(16) C8 0.0225(18) 0.107(4) 0.040(2) -0.027(2) 0.0044(16) -0.006(2) C27 0.052(2) 0.0331(18) 0.0315(18) -0.0023(14) -0.0008(16) 0.0198(17) C26 0.056(2) 0.0225(16) 0.044(2) 0.0024(14) 0.0218(18) 0.0027(16) C10 0.0358(19) 0.047(2) 0.0301(18) -0.0060(15) 0.0136(15) 0.0004(16) C3 0.0224(16) 0.052(2) 0.0225(16) -0.0122(14) -0.0029(13) 0.0030(15) C9 0.056(2) 0.0328(18) 0.0306(18) -0.0052(14) 0.0033(16) -0.0068(16) C17 0.069(3) 0.0279(17) 0.040(2) 0.0088(15) 0.0141(19) 0.0059(18) C23 0.0389(19) 0.0366(18) 0.0240(17) -0.0051(13) -0.0100(14) 0.0086(15) C16 0.054(2) 0.0257(17) 0.042(2) -0.0067(14) 0.0053(17) 0.0045(16) C19 0.0289(18) 0.063(2) 0.0224(17) -0.0005(15) 0.0098(14) -0.0039(16) C7 0.079(3) 0.075(3) 0.049(3) -0.025(2) -0.027(2) 0.052(3) C12 0.0367(19) 0.047(2) 0.0359(19) 0.0004(16) 0.0184(15) -0.0029(16) C6 0.103(4) 0.037(2) 0.030(2) 0.0047(16) 0.010(2) -0.001(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 Fe1 C26 2.040(3) . ? Fe1 C30 2.043(3) . ? Fe1 C23 2.044(3) . ? Fe1 C22 2.045(3) . ? Fe1 C24 2.046(3) . ? Fe1 C25 2.046(3) . ? Fe1 C27 2.047(3) . ? Fe1 C29 2.052(3) . ? Fe1 C28 2.057(3) . ? Fe1 C21 2.066(3) . ? Ti1 N1 1.816(2) . ? Ti1 C20 2.138(3) . ? Ti1 C19 2.152(3) . ? Ti1 C3 2.379(3) . ? Ti1 C4 2.380(3) . ? Ti1 C2 2.431(3) . ? Ti1 C5 2.442(3) . ? Ti1 C1 2.476(3) . ? P1 N1 1.583(2) . ? P1 C21 1.816(3) . ? P1 C11 1.862(3) . ? P1 C15 1.876(3) . ? C25 C24 1.417(4) . ? C25 C21 1.428(4) . ? C21 C22 1.440(4) . ? C15 C17 1.532(4) . ? C15 C16 1.532(4) . ? C15 C18 1.538(5) . ? C14 C11 1.536(4) . ? C29 C28 1.408(5) . ? C29 C30 1.416(5) . ? C28 C27 1.407(5) . ? C22 C23 1.417(5) . ? C1 C2 1.412(5) . ? C1 C5 1.416(4) . ? C1 C6 1.495(5) . ? C30 C26 1.415(5) . ? C4 C5 1.410(4) . ? C4 C3 1.415(4) . ? C4 C9 1.510(4) . ? C5 C10 1.501(4) . ? C11 C13 1.532(4) . ? C11 C12 1.535(4) . ? C24 C23 1.417(5) . ? C2 C3 1.417(5) . ? C2 C7 1.514(5) . ? C8 C3 1.495(5) . ? C27 C26 1.414(5) . ? 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 C26 Fe1 C30 40.55(13) . . ? C26 Fe1 C23 130.23(15) . . ? C30 Fe1 C23 105.10(13) . . ? C26 Fe1 C22 170.35(14) . . ? C30 Fe1 C22 132.39(13) . . ? C23 Fe1 C22 40.55(13) . . ? C26 Fe1 C24 106.15(14) . . ? C30 Fe1 C24 108.71(13) . . ? C23 Fe1 C24 40.55(13) . . ? C22 Fe1 C24 68.28(13) . . ? C26 Fe1 C25 113.04(13) . . ? C30 Fe1 C25 140.61(12) . . ? C23 Fe1 C25 68.18(12) . . ? C22 Fe1 C25 68.31(12) . . ? C24 Fe1 C25 40.53(12) . . ? C26 Fe1 C27 40.48(15) . . ? C30 Fe1 C27 68.02(14) . . ? C23 Fe1 C27 170.67(15) . . ? C22 Fe1 C27 148.79(14) . . ? C24 Fe1 C27 134.16(15) . . ? C25 Fe1 C27 112.72(13) . . ? C26 Fe1 C29 67.97(13) . . ? C30 Fe1 C29 40.45(13) . . ? C23 Fe1 C29 111.57(13) . . ? C22 Fe1 C29 110.77(13) . . ? C24 Fe1 C29 139.92(13) . . ? C25 Fe1 C29 178.90(13) . . ? C27 Fe1 C29 67.71(14) . . ? C26 Fe1 C28 67.69(14) . . ? C30 Fe1 C28 67.69(13) . . ? C23 Fe1 C28 144.50(14) . . ? C22 Fe1 C28 118.01(14) . . ? C24 Fe1 C28 173.71(14) . . ? C25 Fe1 C28 139.63(13) . . ? C27 Fe1 C28 40.11(14) . . ? C29 Fe1 C28 40.09(13) . . ? C26 Fe1 C21 145.67(12) . . ? C30 Fe1 C21 173.22(12) . . ? C23 Fe1 C21 68.67(12) . . ? C22 Fe1 C21 41.01(11) . . ? C24 Fe1 C21 68.57(12) . . ? C25 Fe1 C21 40.65(11) . . ? C27 Fe1 C21 118.48(13) . . ? C29 Fe1 C21 138.25(12) . . ? C28 Fe1 C21 115.61(12) . . ? N1 Ti1 C20 100.42(11) . . ? N1 Ti1 C19 102.79(12) . . ? C20 Ti1 C19 98.65(14) . . ? N1 Ti1 C3 103.16(11) . . ? C20 Ti1 C3 107.58(12) . . ? C19 Ti1 C3 138.67(12) . . ? N1 Ti1 C4 104.68(10) . . ? C20 Ti1 C4 138.50(12) . . ? C19 Ti1 C4 107.19(12) . . ? C3 Ti1 C4 34.60(10) . . ? N1 Ti1 C2 131.25(12) . . ? C20 Ti1 C2 82.07(12) . . ? C19 Ti1 C2 125.18(13) . . ? C3 Ti1 C2 34.24(12) . . ? C4 Ti1 C2 56.54(11) . . ? N1 Ti1 C5 133.79(10) . . ? C20 Ti1 C5 124.55(11) . . ? C19 Ti1 C5 82.13(11) . . ? C3 Ti1 C5 56.75(10) . . ? C4 Ti1 C5 33.98(10) . . ? C2 Ti1 C5 55.75(10) . . ? N1 Ti1 C1 159.07(11) . . ? C20 Ti1 C1 91.58(11) . . ? C19 Ti1 C1 92.15(12) . . ? C3 Ti1 C1 56.53(12) . . ? C4 Ti1 C1 56.24(10) . . ? C2 Ti1 C1 33.43(12) . . ? C5 Ti1 C1 33.45(10) . . ? N1 P1 C21 111.12(13) . . ? N1 P1 C11 110.90(14) . . ? C21 P1 C11 109.25(14) . . ? N1 P1 C15 109.41(13) . . ? C21 P1 C15 102.46(14) . . ? C11 P1 C15 113.42(14) . . ? P1 N1 Ti1 167.58(15) . . ? C24 C25 C21 109.0(3) . . ? C24 C25 Fe1 69.73(17) . . ? C21 C25 Fe1 70.44(16) . . ? C25 C21 C22 106.4(3) . . ? C25 C21 P1 120.8(2) . . ? C22 C21 P1 130.5(2) . . ? C25 C21 Fe1 68.91(16) . . ? C22 C21 Fe1 68.69(16) . . ? P1 C21 Fe1 140.42(16) . . ? C17 C15 C16 109.4(3) . . ? C17 C15 C18 109.4(3) . . ? C16 C15 C18 107.4(3) . . ? C17 C15 P1 114.8(2) . . ? C16 C15 P1 110.0(2) . . ? C18 C15 P1 105.5(2) . . ? C28 C29 C30 107.9(3) . . ? C28 C29 Fe1 70.15(18) . . ? C30 C29 Fe1 69.43(17) . . ? C27 C28 C29 108.4(3) . . ? C27 C28 Fe1 69.57(19) . . ? C29 C28 Fe1 69.76(18) . . ? C23 C22 C21 108.5(3) . . ? C23 C22 Fe1 69.69(18) . . ? C21 C22 Fe1 70.30(16) . . ? C2 C1 C5 107.3(3) . . ? C2 C1 C6 126.3(3) . . ? C5 C1 C6 126.3(3) . . ? C2 C1 Ti1 71.51(17) . . ? C5 C1 Ti1 71.96(16) . . ? C6 C1 Ti1 122.9(2) . . ? C26 C30 C29 107.8(3) . . ? C26 C30 Fe1 69.63(18) . . ? C29 C30 Fe1 70.11(17) . . ? C5 C4 C3 108.4(3) . . ? C5 C4 C9 124.7(3) . . ? C3 C4 C9 126.6(3) . . ? C5 C4 Ti1 75.45(17) . . ? C3 C4 Ti1 72.68(17) . . ? C9 C4 Ti1 122.8(2) . . ? C4 C5 C1 108.3(3) . . ? C4 C5 C10 125.4(3) . . ? C1 C5 C10 126.0(3) . . ? C4 C5 Ti1 70.57(16) . . ? C1 C5 Ti1 74.59(16) . . ? C10 C5 Ti1 125.9(2) . . ? C13 C11 C12 109.4(3) . . ? C13 C11 C14 108.2(3) . . ? C12 C11 C14 109.4(3) . . ? C13 C11 P1 110.3(2) . . ? C12 C11 P1 113.6(2) . . ? C14 C11 P1 105.7(2) . . ? C23 C24 C25 107.9(3) . . ? C23 C24 Fe1 69.65(18) . . ? C25 C24 Fe1 69.74(17) . . ? C1 C2 C3 108.9(3) . . ? C1 C2 C7 125.6(4) . . ? C3 C2 C7 125.1(4) . . ? C1 C2 Ti1 75.06(18) . . ? C3 C2 Ti1 70.89(17) . . ? C7 C2 Ti1 125.6(2) . . ? C28 C27 C26 108.0(3) . . ? C28 C27 Fe1 70.32(19) . . ? C26 C27 Fe1 69.52(19) . . ? C27 C26 C30 107.9(3) . . ? C27 C26 Fe1 70.01(19) . . ? C30 C26 Fe1 69.82(18) . . ? C4 C3 C2 107.1(3) . . ? C4 C3 C8 126.0(3) . . ? C2 C3 C8 126.6(3) . . ? C4 C3 Ti1 72.72(17) . . ? C2 C3 Ti1 74.88(18) . . ? C8 C3 Ti1 122.9(2) . . ? C22 C23 C24 108.2(3) . . ? C22 C23 Fe1 69.77(17) . . ? C24 C23 Fe1 69.80(18) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.670 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.087 #===end data_[(?5-C5Ph5)Fe(?5-C5H4PtBu2NSiMe3)] _database_code_depnum_ccdc_archive 'CCDC 747509' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C51 H56 Fe N P Si' _chemical_formula_weight 797.88 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' Fe Fe 0.3463 0.8444 '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 18.467(4) _cell_length_b 12.868(3) _cell_length_c 20.237(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.06(3) _cell_angle_gamma 90.00 _cell_volume 4356.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 40834 _diffrn_reflns_av_R_equivalents 0.1036 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9951 _reflns_number_gt 5153 _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 Rfactors 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^)+(0.0706P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 9951 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1493 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Fe1 Fe 0.26318(3) 0.54404(3) 0.09957(2) 0.02476(14) Uani 1 1 d . . . P1 P 0.42015(5) 0.73892(7) 0.10085(4) 0.0298(2) Uani 1 1 d . . . Si1 Si 0.42081(6) 0.73245(9) -0.05622(5) 0.0421(3) Uani 1 1 d . . . N1 N 0.41204(16) 0.7296(2) 0.02254(13) 0.0336(7) Uani 1 1 d . . . C1 C 0.36980(17) 0.6307(2) 0.12246(15) 0.0252(7) Uani 1 1 d . . . C2 C 0.36774(17) 0.5345(3) 0.08696(16) 0.0290(8) Uani 1 1 d . . . H2A H 0.3714 0.5267 0.0403 0.035 Uiso 1 1 calc R . . C3 C 0.36136(18) 0.4517(3) 0.13029(16) 0.0316(8) Uani 1 1 d . . . H3A H 0.3616 0.3774 0.1197 0.038 Uiso 1 1 calc R . . C4 C 0.35712(18) 0.4954(3) 0.19281(17) 0.0330(8) Uani 1 1 d . . . H4A H 0.3532 0.4567 0.2329 0.040 Uiso 1 1 calc R . . C5 C 0.36073(18) 0.6050(3) 0.18776(16) 0.0310(8) Uani 1 1 d . . . H5A H 0.3581 0.6550 0.2232 0.037 Uiso 1 1 calc R . . C6 C 0.17094(17) 0.4981(2) 0.00325(15) 0.0247(7) Uani 1 1 d . . . C7 C 0.17611(17) 0.4314(2) 0.06210(15) 0.0245(7) Uani 1 1 d . . . C8 C 0.16650(17) 0.4953(3) 0.11577(15) 0.0257(7) Uani 1 1 d . . . C9 C 0.15358(17) 0.5996(2) 0.09003(15) 0.0234(7) Uani 1 1 d . . . C10 C 0.15596(17) 0.6020(2) 0.01961(15) 0.0238(7) Uani 1 1 d . . . C11 C 0.17471(18) 0.4594(2) -0.06504(15) 0.0264(7) Uani 1 1 d . . . C12 C 0.1126(2) 0.4801(3) -0.13285(16) 0.0355(8) Uani 1 1 d . . . H12A H 0.0702 0.5219 -0.1361 0.043 Uiso 1 1 calc R . . C13 C 0.1138(3) 0.4388(3) -0.19533(17) 0.0478(10) Uani 1 1 d . . . H13A H 0.0714 0.4518 -0.2402 0.057 Uiso 1 1 calc R . . C14 C 0.1771(3) 0.3783(3) -0.1921(2) 0.0546(12) Uani 1 1 d . . . H14A H 0.1782 0.3521 -0.2345 0.066 Uiso 1 1 calc R . . C15 C 0.2381(2) 0.3578(3) -0.1253(2) 0.0523(11) Uani 1 1 d . . . H15A H 0.2804 0.3160 -0.1225 0.063 Uiso 1 1 calc R . . C16 C 0.2380(2) 0.3976(3) -0.06228(18) 0.0381(9) Uani 1 1 d . . . H16A H 0.2804 0.3833 -0.0176 0.046 Uiso 1 1 calc R . . C21 C 0.17881(18) 0.3161(3) 0.06382(16) 0.0287(8) Uani 1 1 d . . . C22 C 0.2256(2) 0.2601(3) 0.12690(18) 0.0339(8) Uani 1 1 d . . . H22A H 0.2615 0.2953 0.1678 0.041 Uiso 1 1 calc R . . C23 C 0.2192(2) 0.1539(3) 0.1292(2) 0.0415(9) Uani 1 1 d . . . H23A H 0.2510 0.1181 0.1716 0.050 Uiso 1 1 calc R . . C24 C 0.1660(2) 0.0994(3) 0.0693(2) 0.0454(10) Uani 1 1 d . . . H24A H 0.1614 0.0277 0.0714 0.054 Uiso 1 1 calc R . . C25 C 0.1199(2) 0.1535(3) 0.0062(2) 0.0436(9) Uani 1 1 d . . . H25A H 0.0843 0.1177 -0.0345 0.052 Uiso 1 1 calc R . . C26 C 0.1264(2) 0.2600(3) 0.00340(17) 0.0335(8) Uani 1 1 d . . . H26A H 0.0953 0.2951 -0.0395 0.040 Uiso 1 1 calc R . . C31 C 0.15836(18) 0.4564(2) 0.18165(15) 0.0266(7) Uani 1 1 d . . . C32 C 0.09821(19) 0.3849(3) 0.17285(17) 0.0327(8) Uani 1 1 d . . . H32A H 0.0659 0.3599 0.1265 0.039 Uiso 1 1 calc R . . C33 C 0.0860(2) 0.3509(3) 0.23229(18) 0.0397(9) Uani 1 1 d . . . H33A H 0.0452 0.3039 0.2256 0.048 Uiso 1 1 calc R . . C34 C 0.1341(2) 0.3862(3) 0.30118(18) 0.0435(10) Uani 1 1 d . . . H34A H 0.1261 0.3627 0.3411 0.052 Uiso 1 1 calc R . . C35 C 0.1942(2) 0.4568(3) 0.31113(17) 0.0393(9) Uani 1 1 d . . . H35A H 0.2270 0.4802 0.3578 0.047 Uiso 1 1 calc R . . C36 C 0.2059(2) 0.4931(3) 0.25158(16) 0.0334(8) Uani 1 1 d . . . H36A H 0.2456 0.5420 0.2584 0.040 Uiso 1 1 calc R . . C41 C 0.12921(18) 0.6838(3) 0.12708(16) 0.0276(7) Uani 1 1 d . . . C42 C 0.1681(2) 0.7778(3) 0.14806(19) 0.0451(10) Uani 1 1 d . . . H42A H 0.2121 0.7918 0.1384 0.054 Uiso 1 1 calc R . . C43 C 0.1424(2) 0.8520(3) 0.1834(2) 0.0549(11) Uani 1 1 d . . . H43A H 0.1692 0.9151 0.1974 0.066 Uiso 1 1 calc R . . C44 C 0.0772(2) 0.8313(3) 0.1976(2) 0.0491(10) Uani 1 1 d . . . H44A H 0.0600 0.8805 0.2214 0.059 Uiso 1 1 calc R . . C45 C 0.0378(2) 0.7398(3) 0.17702(18) 0.0382(9) Uani 1 1 d . . . H45A H -0.0066 0.7266 0.1862 0.046 Uiso 1 1 calc R . . C46 C 0.06396(19) 0.6658(3) 0.14226(16) 0.0319(8) Uani 1 1 d . . . H46A H 0.0371 0.6027 0.1289 0.038 Uiso 1 1 calc R . . C51 C 0.13608(18) 0.6922(2) -0.03010(15) 0.0258(7) Uani 1 1 d . . . C52 C 0.07299(19) 0.7581(3) -0.03786(16) 0.0340(8) Uani 1 1 d . . . H52A H 0.0454 0.7471 -0.0092 0.041 Uiso 1 1 calc R . . C53 C 0.0505(2) 0.8395(3) -0.08742(19) 0.0443(9) Uani 1 1 d . . . H53A H 0.0082 0.8825 -0.0919 0.053 Uiso 1 1 calc R . . C54 C 0.0910(2) 0.8564(3) -0.12994(19) 0.0450(10) Uani 1 1 d . . . H54A H 0.0764 0.9112 -0.1630 0.054 Uiso 1 1 calc R . . C55 C 0.1537(2) 0.7917(3) -0.12345(17) 0.0376(9) Uani 1 1 d . . . H55A H 0.1806 0.8029 -0.1526 0.045 Uiso 1 1 calc R . . C56 C 0.17636(19) 0.7111(3) -0.07413(16) 0.0322(8) Uani 1 1 d . . . H56A H 0.2188 0.6686 -0.0700 0.039 Uiso 1 1 calc R . . C60 C 0.5260(2) 0.7162(3) 0.16927(17) 0.0382(9) Uani 1 1 d . . . C61 C 0.5409(2) 0.7319(3) 0.24903(18) 0.0514(11) Uani 1 1 d . . . H61A H 0.5961 0.7183 0.2801 0.077 Uiso 1 1 calc R . . H61B H 0.5078 0.6851 0.2610 0.077 Uiso 1 1 calc R . . H61C H 0.5282 0.8022 0.2560 0.077 Uiso 1 1 calc R . . C62 C 0.5486(2) 0.6044(3) 0.1599(2) 0.0520(10) Uani 1 1 d . . . H62A H 0.6026 0.5909 0.1943 0.078 Uiso 1 1 calc R . . H62B H 0.5442 0.5952 0.1113 0.078 Uiso 1 1 calc R . . H62C H 0.5132 0.5570 0.1683 0.078 Uiso 1 1 calc R . . C63 C 0.5823(2) 0.7883(3) 0.15150(19) 0.0467(10) Uani 1 1 d . . . H63A H 0.6366 0.7767 0.1861 0.070 Uiso 1 1 calc R . . H63B H 0.5681 0.8595 0.1542 0.070 Uiso 1 1 calc R . . H63C H 0.5773 0.7737 0.1032 0.070 Uiso 1 1 calc R . . C64 C 0.38073(19) 0.8649(3) 0.11675(17) 0.0346(8) Uani 1 1 d . . . C65 C 0.3729(2) 0.8748(3) 0.18907(19) 0.0516(11) Uani 1 1 d . . . H65A H 0.3516 0.9420 0.1917 0.077 Uiso 1 1 calc R . . H65B H 0.4245 0.8668 0.2291 0.077 Uiso 1 1 calc R . . H65C H 0.3376 0.8218 0.1916 0.077 Uiso 1 1 calc R . . C66 C 0.4321(2) 0.9562(3) 0.1113(2) 0.0579(11) Uani 1 1 d . . . H66A H 0.4107 1.0205 0.1194 0.087 Uiso 1 1 calc R . . H66B H 0.4315 0.9569 0.0636 0.087 Uiso 1 1 calc R . . H66C H 0.4861 0.9481 0.1474 0.087 Uiso 1 1 calc R . . C67 C 0.2980(2) 0.8759(3) 0.05293(19) 0.0473(10) Uani 1 1 d . . . H67A H 0.2739 0.9398 0.0578 0.071 Uiso 1 1 calc R . . H67B H 0.2649 0.8186 0.0533 0.071 Uiso 1 1 calc R . . H67C H 0.3035 0.8762 0.0078 0.071 Uiso 1 1 calc R . . C68 C 0.3490(3) 0.6418(4) -0.1246(2) 0.0769(15) Uani 1 1 d . . . H68A H 0.2957 0.6574 -0.1308 0.115 Uiso 1 1 calc R . . H68B H 0.3621 0.5715 -0.1078 0.115 Uiso 1 1 calc R . . H68C H 0.3524 0.6497 -0.1704 0.115 Uiso 1 1 calc R . . C69 C 0.5226(3) 0.6961(5) -0.0474(2) 0.0942(19) Uani 1 1 d . . . H69A H 0.5616 0.7420 -0.0134 0.141 Uiso 1 1 calc R . . H69B H 0.5241 0.7019 -0.0941 0.141 Uiso 1 1 calc R . . H69C H 0.5343 0.6258 -0.0303 0.141 Uiso 1 1 calc R . . C70 C 0.4001(3) 0.8645(4) -0.0980(2) 0.0839(16) Uani 1 1 d . . . H70A H 0.4356 0.9139 -0.0643 0.126 Uiso 1 1 calc R . . H70B H 0.3458 0.8834 -0.1095 0.126 Uiso 1 1 calc R . . H70C H 0.4082 0.8641 -0.1419 0.126 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 Fe1 0.0226(2) 0.0269(3) 0.0253(2) 0.0014(2) 0.01065(19) 0.0007(2) P1 0.0289(5) 0.0324(6) 0.0305(4) -0.0033(4) 0.0151(4) -0.0030(4) Si1 0.0393(6) 0.0579(8) 0.0357(5) 0.0017(5) 0.0222(5) 0.0030(5) N1 0.0402(17) 0.0339(18) 0.0329(14) 0.0007(12) 0.0215(13) 0.0006(14) C1 0.0204(16) 0.027(2) 0.0272(16) -0.0028(14) 0.0096(13) -0.0009(14) C2 0.0233(17) 0.033(2) 0.0318(17) 0.0010(15) 0.0128(14) 0.0013(15) C3 0.0225(17) 0.029(2) 0.0391(18) -0.0005(16) 0.0089(15) 0.0045(15) C4 0.0211(18) 0.040(2) 0.0338(18) 0.0085(16) 0.0076(15) 0.0016(16) C5 0.0283(19) 0.036(2) 0.0273(17) -0.0008(15) 0.0108(14) -0.0015(16) C6 0.0224(17) 0.0252(19) 0.0285(16) 0.0022(14) 0.0127(14) 0.0017(14) C7 0.0214(17) 0.025(2) 0.0256(16) 0.0025(13) 0.0084(13) 0.0020(14) C8 0.0209(17) 0.030(2) 0.0280(16) 0.0021(14) 0.0118(14) 0.0009(14) C9 0.0206(16) 0.025(2) 0.0270(16) 0.0001(14) 0.0119(13) -0.0001(14) C10 0.0206(16) 0.026(2) 0.0261(16) 0.0011(14) 0.0107(13) 0.0002(14) C11 0.0285(18) 0.0267(19) 0.0264(16) -0.0015(14) 0.0140(14) -0.0064(15) C12 0.042(2) 0.029(2) 0.0328(18) 0.0006(15) 0.0135(16) -0.0047(16) C13 0.073(3) 0.039(3) 0.0229(18) -0.0026(16) 0.0125(19) -0.019(2) C14 0.095(3) 0.043(3) 0.046(2) -0.0161(19) 0.049(3) -0.024(2) C15 0.061(3) 0.052(3) 0.060(3) -0.019(2) 0.041(2) -0.011(2) C16 0.033(2) 0.043(2) 0.042(2) -0.0066(17) 0.0209(17) -0.0044(17) C21 0.0239(17) 0.032(2) 0.0353(18) 0.0034(15) 0.0173(15) 0.0032(15) C22 0.033(2) 0.029(2) 0.0415(19) 0.0030(16) 0.0174(16) 0.0027(16) C23 0.040(2) 0.032(2) 0.054(2) 0.0108(18) 0.0216(19) 0.0085(18) C24 0.054(3) 0.023(2) 0.069(3) 0.003(2) 0.036(2) 0.0028(19) C25 0.047(2) 0.032(2) 0.055(2) -0.0087(19) 0.025(2) -0.0073(19) C26 0.034(2) 0.032(2) 0.0343(18) 0.0020(15) 0.0150(16) 0.0005(16) C31 0.0256(17) 0.027(2) 0.0300(16) 0.0042(14) 0.0144(14) 0.0065(15) C32 0.034(2) 0.031(2) 0.0356(18) -0.0004(15) 0.0174(16) 0.0008(17) C33 0.051(2) 0.030(2) 0.052(2) 0.0051(17) 0.035(2) -0.0008(18) C34 0.060(3) 0.045(3) 0.035(2) 0.0093(17) 0.0293(19) 0.004(2) C35 0.056(2) 0.037(2) 0.0282(17) 0.0020(16) 0.0200(17) 0.0056(19) C36 0.038(2) 0.031(2) 0.0345(18) -0.0003(15) 0.0192(16) -0.0007(16) C41 0.0291(18) 0.027(2) 0.0272(16) 0.0027(14) 0.0128(14) 0.0011(16) C42 0.051(2) 0.039(3) 0.057(2) -0.0063(19) 0.034(2) -0.010(2) C43 0.068(3) 0.037(3) 0.072(3) -0.022(2) 0.040(2) -0.014(2) C44 0.060(3) 0.039(3) 0.060(2) -0.0164(19) 0.037(2) -0.002(2) C45 0.042(2) 0.036(2) 0.045(2) -0.0006(17) 0.0270(18) 0.0041(18) C46 0.0325(19) 0.030(2) 0.0362(18) -0.0018(15) 0.0172(16) 0.0024(16) C51 0.0259(17) 0.027(2) 0.0227(15) -0.0002(14) 0.0086(13) 0.0011(15) C52 0.033(2) 0.036(2) 0.0325(18) 0.0017(16) 0.0136(16) 0.0026(16) C53 0.039(2) 0.037(2) 0.050(2) 0.0090(18) 0.0118(18) 0.0043(18) C54 0.043(2) 0.039(3) 0.042(2) 0.0147(17) 0.0079(18) -0.0057(19) C55 0.042(2) 0.036(2) 0.0337(18) 0.0058(16) 0.0156(17) -0.0065(18) C56 0.0332(19) 0.030(2) 0.0345(18) -0.0004(15) 0.0152(16) -0.0016(16) C60 0.034(2) 0.047(3) 0.0333(18) -0.0097(16) 0.0147(16) -0.0069(18) C61 0.030(2) 0.076(3) 0.040(2) -0.0054(19) 0.0081(17) -0.012(2) C62 0.032(2) 0.055(3) 0.056(2) -0.006(2) 0.0056(18) 0.0037(19) C63 0.033(2) 0.059(3) 0.050(2) -0.0064(19) 0.0198(18) -0.0070(19) C64 0.033(2) 0.036(2) 0.0388(18) -0.0094(16) 0.0186(16) -0.0055(16) C65 0.057(3) 0.052(3) 0.051(2) -0.0164(19) 0.028(2) 0.003(2) C66 0.059(3) 0.031(2) 0.094(3) -0.012(2) 0.043(2) -0.011(2) C67 0.042(2) 0.045(3) 0.056(2) -0.0096(19) 0.0223(19) 0.0069(19) C68 0.088(4) 0.103(4) 0.054(3) -0.027(3) 0.044(3) -0.018(3) C69 0.064(3) 0.170(6) 0.063(3) -0.010(3) 0.041(3) 0.030(3) C70 0.117(4) 0.085(4) 0.056(3) 0.024(3) 0.043(3) 0.002(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 Fe1 C3 2.033(3) . ? Fe1 C8 2.045(3) . ? Fe1 C4 2.047(3) . ? Fe1 C2 2.056(3) . ? Fe1 C7 2.056(3) . ? Fe1 C6 2.059(3) . ? Fe1 C9 2.077(3) . ? Fe1 C5 2.079(3) . ? Fe1 C10 2.093(3) . ? Fe1 C1 2.136(3) . ? P1 N1 1.532(2) . ? P1 C1 1.827(3) . ? P1 C64 1.860(3) . ? P1 C60 1.880(4) . ? Si1 N1 1.669(2) . ? Si1 C70 1.864(4) . ? Si1 C68 1.866(4) . ? Si1 C69 1.870(4) . ? C1 C2 1.424(4) . ? C1 C5 1.439(4) . ? C2 C3 1.417(4) . ? C3 C4 1.417(4) . ? C4 C5 1.417(5) . ? C6 C10 1.432(4) . ? C6 C7 1.438(4) . ? C6 C11 1.498(4) . ? C7 C8 1.432(4) . ? C7 C21 1.484(4) . ? C8 C9 1.422(4) . ? C8 C31 1.490(4) . ? C9 C10 1.444(4) . ? C9 C41 1.492(4) . ? C10 C51 1.477(4) . ? C11 C12 1.391(4) . ? C11 C16 1.395(4) . ? C12 C13 1.380(5) . ? C13 C14 1.382(5) . ? C14 C15 1.371(6) . ? C15 C16 1.374(5) . ? C21 C26 1.397(4) . ? C21 C22 1.400(4) . ? C22 C23 1.375(5) . ? C23 C24 1.384(5) . ? C24 C25 1.385(5) . ? C25 C26 1.380(5) . ? C31 C32 1.394(4) . ? C31 C36 1.394(4) . ? C32 C33 1.386(4) . ? C33 C34 1.375(5) . ? C34 C35 1.382(5) . ? C35 C36 1.392(4) . ? C41 C42 1.378(5) . ? C41 C46 1.383(4) . ? C42 C43 1.391(5) . ? C43 C44 1.378(5) . ? C44 C45 1.353(5) . ? C45 C46 1.387(4) . ? C51 C52 1.394(4) . ? C51 C56 1.403(4) . ? C52 C53 1.387(5) . ? C53 C54 1.376(5) . ? C54 C55 1.386(5) . ? C55 C56 1.377(4) . ? C60 C62 1.531(5) . ? C60 C61 1.532(4) . ? C60 C63 1.546(5) . ? C64 C67 1.533(5) . ? C64 C65 1.536(4) . ? C64 C66 1.544(5) . ? 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 C3 Fe1 C8 119.85(13) . . ? C3 Fe1 C4 40.65(12) . . ? C8 Fe1 C4 102.42(12) . . ? C3 Fe1 C2 40.54(12) . . ? C8 Fe1 C2 158.61(13) . . ? C4 Fe1 C2 67.81(12) . . ? C3 Fe1 C7 99.07(13) . . ? C8 Fe1 C7 40.86(12) . . ? C4 Fe1 C7 110.46(13) . . ? C2 Fe1 C7 122.76(12) . . ? C3 Fe1 C6 113.25(13) . . ? C8 Fe1 C6 68.61(11) . . ? C4 Fe1 C6 145.44(14) . . ? C2 Fe1 C6 108.02(12) . . ? C7 Fe1 C6 40.91(11) . . ? C3 Fe1 C9 159.64(12) . . ? C8 Fe1 C9 40.36(12) . . ? C4 Fe1 C9 127.09(12) . . ? C2 Fe1 C9 159.81(12) . . ? C7 Fe1 C9 68.23(12) . . ? C6 Fe1 C9 68.15(12) . . ? C3 Fe1 C5 67.77(13) . . ? C8 Fe1 C5 118.42(12) . . ? C4 Fe1 C5 40.18(13) . . ? C2 Fe1 C5 67.11(12) . . ? C7 Fe1 C5 147.19(12) . . ? C6 Fe1 C5 171.81(12) . . ? C9 Fe1 C5 113.97(12) . . ? C3 Fe1 C10 150.92(12) . . ? C8 Fe1 C10 68.23(11) . . ? C4 Fe1 C10 167.58(12) . . ? C2 Fe1 C10 123.77(12) . . ? C7 Fe1 C10 68.29(12) . . ? C6 Fe1 C10 40.35(12) . . ? C9 Fe1 C10 40.53(11) . . ? C5 Fe1 C10 136.16(13) . . ? C3 Fe1 C1 67.55(13) . . ? C8 Fe1 C1 155.83(11) . . ? C4 Fe1 C1 67.43(13) . . ? C2 Fe1 C1 39.65(12) . . ? C7 Fe1 C1 162.37(11) . . ? C6 Fe1 C1 132.24(11) . . ? C9 Fe1 C1 127.81(12) . . ? C5 Fe1 C1 39.90(11) . . ? C10 Fe1 C1 117.69(12) . . ? N1 P1 C1 110.55(14) . . ? N1 P1 C64 111.93(15) . . ? C1 P1 C64 110.28(14) . . ? N1 P1 C60 111.41(15) . . ? C1 P1 C60 100.43(15) . . ? C64 P1 C60 111.69(15) . . ? N1 Si1 C70 111.70(17) . . ? N1 Si1 C68 111.63(17) . . ? C70 Si1 C68 106.8(2) . . ? N1 Si1 C69 113.79(17) . . ? C70 Si1 C69 106.0(3) . . ? C68 Si1 C69 106.5(2) . . ? P1 N1 Si1 168.3(2) . . ? C2 C1 C5 105.9(3) . . ? C2 C1 P1 116.7(2) . . ? C5 C1 P1 131.6(2) . . ? C2 C1 Fe1 67.13(17) . . ? C5 C1 Fe1 67.91(17) . . ? P1 C1 Fe1 149.52(17) . . ? C3 C2 C1 109.5(3) . . ? C3 C2 Fe1 68.85(17) . . ? C1 C2 Fe1 73.22(17) . . ? C2 C3 C4 107.7(3) . . ? C2 C3 Fe1 70.60(18) . . ? C4 C3 Fe1 70.20(18) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Fe1 69.14(18) . . ? C5 C4 Fe1 71.14(18) . . ? C4 C5 C1 108.8(3) . . ? C4 C5 Fe1 68.68(18) . . ? C1 C5 Fe1 72.19(17) . . ? C10 C6 C7 108.5(2) . . ? C10 C6 C11 127.8(3) . . ? C7 C6 C11 123.6(3) . . ? C10 C6 Fe1 71.12(17) . . ? C7 C6 Fe1 69.45(17) . . ? C11 C6 Fe1 128.8(2) . . ? C8 C7 C6 107.4(3) . . ? C8 C7 C21 124.7(3) . . ? C6 C7 C21 127.3(3) . . ? C8 C7 Fe1 69.17(17) . . ? C6 C7 Fe1 69.64(17) . . ? C21 C7 Fe1 133.0(2) . . ? C9 C8 C7 108.6(2) . . ? C9 C8 C31 125.4(3) . . ? C7 C8 C31 125.3(3) . . ? C9 C8 Fe1 71.00(17) . . ? C7 C8 Fe1 69.97(16) . . ? C31 C8 Fe1 132.2(2) . . ? C8 C9 C10 108.1(3) . . ? C8 C9 C41 122.7(2) . . ? C10 C9 C41 128.4(3) . . ? C8 C9 Fe1 68.64(16) . . ? C10 C9 Fe1 70.35(16) . . ? C41 C9 Fe1 133.8(2) . . ? C6 C10 C9 107.3(3) . . ? C6 C10 C51 126.4(2) . . ? C9 C10 C51 125.9(3) . . ? C6 C10 Fe1 68.53(16) . . ? C9 C10 Fe1 69.12(16) . . ? C51 C10 Fe1 133.4(2) . . ? C12 C11 C16 118.4(3) . . ? C12 C11 C6 120.3(3) . . ? C16 C11 C6 121.2(3) . . ? C13 C12 C11 120.2(3) . . ? C12 C13 C14 121.0(3) . . ? C15 C14 C13 118.7(3) . . ? C14 C15 C16 121.4(4) . . ? C15 C16 C11 120.3(3) . . ? C26 C21 C22 117.6(3) . . ? C26 C21 C7 119.5(3) . . ? C22 C21 C7 122.5(3) . . ? C23 C22 C21 120.9(3) . . ? C22 C23 C24 120.8(3) . . ? C23 C24 C25 119.0(3) . . ? C26 C25 C24 120.5(3) . . ? C25 C26 C21 121.2(3) . . ? C32 C31 C36 118.6(3) . . ? C32 C31 C8 118.9(3) . . ? C36 C31 C8 122.4(3) . . ? C33 C32 C31 120.8(3) . . ? C34 C33 C32 120.2(3) . . ? C33 C34 C35 120.0(3) . . ? C34 C35 C36 120.3(3) . . ? C35 C36 C31 120.2(3) . . ? C42 C41 C46 117.9(3) . . ? C42 C41 C9 124.3(3) . . ? C46 C41 C9 117.8(3) . . ? C41 C42 C43 121.0(3) . . ? C44 C43 C42 119.5(4) . . ? C45 C44 C43 120.5(3) . . ? C44 C45 C46 119.8(3) . . ? C41 C46 C45 121.4(3) . . ? C52 C51 C56 117.8(3) . . ? C52 C51 C10 120.6(3) . . ? C56 C51 C10 121.5(3) . . ? C53 C52 C51 121.4(3) . . ? C54 C53 C52 119.7(3) . . ? C53 C54 C55 120.0(3) . . ? C56 C55 C54 120.5(3) . . ? C55 C56 C51 120.7(3) . . ? C62 C60 C61 108.5(3) . . ? C62 C60 C63 106.9(3) . . ? C61 C60 C63 109.1(3) . . ? C62 C60 P1 107.9(2) . . ? C61 C60 P1 115.0(2) . . ? C63 C60 P1 109.1(2) . . ? C67 C64 C65 109.4(3) . . ? C67 C64 C66 107.0(3) . . ? C65 C64 C66 108.3(3) . . ? C67 C64 P1 104.9(2) . . ? C65 C64 P1 116.0(3) . . ? C66 C64 P1 110.7(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.474 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.076 #===end data_[TiCp{N=P(?5-C5H4)Fe(?5-C5Ph5)PtBu2}Cl2] _database_code_depnum_ccdc_archive 'CCDC 747510' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C56.50 H56 Cl2 Fe N P Ti' _chemical_formula_weight 954.64 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' Fe Fe 0.3463 0.8444 '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 14.3943(14) _cell_length_b 16.9970(17) _cell_length_c 21.197(2) _cell_angle_alpha 72.4480(10) _cell_angle_beta 89.9460(10) _cell_angle_gamma 81.3970(10) _cell_volume 4883.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.791686 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 298(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 47239 _diffrn_reflns_av_R_equivalents 0.1262 _diffrn_reflns_av_sigmaI/netI 0.1892 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17148 _reflns_number_gt 7349 _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 Rfactors 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^)+(0.0646P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 17148 _refine_ls_number_parameters 1126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1816 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _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 Fe1 Fe 0.90799(6) 1.23975(5) 0.03250(4) 0.0327(2) Uani 1 1 d . . . Fe2 Fe 0.47270(5) 0.79857(5) 0.46252(4) 0.0304(2) Uani 1 1 d . . . Ti1 Ti 0.60728(8) 1.14052(7) 0.21056(5) 0.0419(3) Uani 1 1 d . . . Ti2 Ti 0.14575(7) 0.88144(7) 0.27544(5) 0.0387(3) Uani 1 1 d . . . Cl1 Cl 0.49969(13) 1.04896(12) 0.22244(9) 0.0718(6) Uani 1 1 d . . . Cl2 Cl 0.50984(13) 1.26632(11) 0.18045(9) 0.0678(6) Uani 1 1 d . . . Cl3 Cl 0.01542(12) 0.98462(11) 0.25613(8) 0.0638(5) Uani 1 1 d . . . Cl4 Cl 0.07375(12) 0.76542(11) 0.31081(9) 0.0593(5) Uani 1 1 d . . . P1 P 0.69512(11) 1.12483(10) 0.06775(8) 0.0385(4) Uani 1 1 d . . . P2 P 0.22182(10) 0.91114(10) 0.41389(7) 0.0335(4) Uani 1 1 d . . . N1 N 0.6601(3) 1.1376(3) 0.1365(2) 0.0394(13) Uani 1 1 d . . . N2 N 0.1992(3) 0.8875(3) 0.3486(2) 0.0309(12) Uani 1 1 d . . . C1 C 0.6436(6) 1.1817(6) 0.3055(4) 0.077(3) Uani 1 1 d . . . H1A H 0.6141 1.2322 0.3155 0.093 Uiso 1 1 calc R . . C2 C 0.7253(7) 1.1744(7) 0.2689(4) 0.085(3) Uani 1 1 d . . . H2A H 0.7639 1.2181 0.2509 0.102 Uiso 1 1 calc R . . C3 C 0.7495(6) 1.0906(7) 0.2743(4) 0.081(3) Uani 1 1 d . . . H3A H 0.8080 1.0653 0.2598 0.097 Uiso 1 1 calc R . . C4 C 0.6819(6) 1.0470(5) 0.3096(3) 0.075(2) Uani 1 1 d . . . H4A H 0.6847 0.9862 0.3242 0.090 Uiso 1 1 calc R . . C5 C 0.6188(6) 1.1037(6) 0.3295(3) 0.069(2) Uani 1 1 d . . . H5A H 0.5672 1.0896 0.3589 0.083 Uiso 1 1 calc R . . C6 C 0.7144(5) 1.0100(4) 0.0773(4) 0.0546(19) Uani 1 1 d . . . C7 C 0.6220(6) 0.9763(5) 0.0821(4) 0.092(3) Uani 1 1 d . . . H7A H 0.6340 0.9177 0.0869 0.138 Uiso 1 1 calc R . . H7B H 0.5833 1.0051 0.0426 0.138 Uiso 1 1 calc R . . H7C H 0.5901 0.9849 0.1199 0.138 Uiso 1 1 calc R . . C8 C 0.7695(6) 0.9668(4) 0.1439(5) 0.111(3) Uani 1 1 d . . . H8A H 0.7813 0.9075 0.1512 0.166 Uiso 1 1 calc R . . H8B H 0.7335 0.9785 0.1790 0.166 Uiso 1 1 calc R . . H8C H 0.8283 0.9873 0.1430 0.166 Uiso 1 1 calc R . . C9 C 0.7677(7) 0.9871(5) 0.0220(5) 0.121(4) Uani 1 1 d . . . H9A H 0.7749 0.9277 0.0302 0.182 Uiso 1 1 calc R . . H9B H 0.8287 1.0039 0.0204 0.182 Uiso 1 1 calc R . . H9C H 0.7335 1.0150 -0.0195 0.182 Uiso 1 1 calc R . . C10 C 0.6072(4) 1.1887(5) 0.0014(3) 0.0483(18) Uani 1 1 d . . . C11 C 0.5073(5) 1.1679(5) 0.0180(4) 0.083(3) Uani 1 1 d . . . H11A H 0.4633 1.2019 -0.0171 0.124 Uiso 1 1 calc R . . H11B H 0.4900 1.1790 0.0586 0.124 Uiso 1 1 calc R . . H11C H 0.5066 1.1100 0.0229 0.124 Uiso 1 1 calc R . . C12 C 0.6321(5) 1.1792(5) -0.0667(3) 0.087(3) Uani 1 1 d . . . H12A H 0.5847 1.2133 -0.0994 0.131 Uiso 1 1 calc R . . H12B H 0.6351 1.1218 -0.0650 0.131 Uiso 1 1 calc R . . H12C H 0.6920 1.1965 -0.0782 0.131 Uiso 1 1 calc R . . C13 C 0.6060(5) 1.2778(4) 0.0013(3) 0.067(2) Uani 1 1 d . . . H13A H 0.5614 1.3145 -0.0324 0.101 Uiso 1 1 calc R . . H13B H 0.6674 1.2928 -0.0077 0.101 Uiso 1 1 calc R . . H13C H 0.5883 1.2828 0.0437 0.101 Uiso 1 1 calc R . . C14 C 0.8112(4) 1.1521(3) 0.0508(3) 0.0344(15) Uani 1 1 d . . . C15 C 0.8667(4) 1.1496(3) -0.0048(3) 0.0407(16) Uani 1 1 d . . . H15A H 0.8428 1.1586 -0.0501 0.049 Uiso 1 1 calc R . . C16 C 0.9620(4) 1.1296(4) 0.0178(3) 0.0482(18) Uani 1 1 d . . . H16A H 1.0154 1.1214 -0.0095 0.058 Uiso 1 1 calc R . . C17 C 0.9687(4) 1.1215(4) 0.0861(3) 0.0486(18) Uani 1 1 d . . . H17A H 1.0265 1.1063 0.1143 0.058 Uiso 1 1 calc R . . C18 C 0.8765(4) 1.1368(3) 0.1063(3) 0.0401(16) Uani 1 1 d . . . H18A H 0.8593 1.1361 0.1512 0.048 Uiso 1 1 calc R . . C19 C 0.8960(4) 1.3570(4) -0.0379(3) 0.0337(15) Uani 1 1 d . . . C20 C 0.8596(4) 1.3655(3) 0.0230(3) 0.0368(15) Uani 1 1 d . . . C21 C 0.9324(4) 1.3310(3) 0.0748(3) 0.0339(15) Uani 1 1 d . . . C22 C 1.0150(4) 1.3029(4) 0.0445(3) 0.0364(15) Uani 1 1 d . . . C23 C 0.9926(4) 1.3191(3) -0.0249(3) 0.0329(14) Uani 1 1 d . . . C24 C 0.8507(4) 1.3952(4) -0.1054(3) 0.0385(16) Uani 1 1 d . . . C25 C 0.7717(5) 1.3727(5) -0.1264(3) 0.068(2) Uani 1 1 d . . . H25A H 0.7441 1.3304 -0.0978 0.082 Uiso 1 1 calc R . . C26 C 0.7318(6) 1.4127(5) -0.1903(4) 0.082(3) Uani 1 1 d . . . H26A H 0.6791 1.3958 -0.2045 0.098 Uiso 1 1 calc R . . C27 C 0.7704(7) 1.4766(6) -0.2320(4) 0.087(3) Uani 1 1 d . . . H27A H 0.7424 1.5048 -0.2739 0.104 Uiso 1 1 calc R . . C28 C 0.8488(6) 1.4986(5) -0.2123(4) 0.074(2) Uani 1 1 d . . . H28A H 0.8759 1.5411 -0.2411 0.089 Uiso 1 1 calc R . . C29 C 0.8893(5) 1.4584(4) -0.1497(3) 0.0511(18) Uani 1 1 d . . . H29A H 0.9437 1.4741 -0.1370 0.061 Uiso 1 1 calc R . . C30 C 0.7673(4) 1.4137(4) 0.0305(3) 0.0397(16) Uani 1 1 d . . . C31 C 0.7401(5) 1.4939(4) -0.0117(4) 0.064(2) Uani 1 1 d . . . H31A H 0.7779 1.5152 -0.0464 0.077 Uiso 1 1 calc R . . C32 C 0.6590(6) 1.5427(5) -0.0036(4) 0.088(3) Uani 1 1 d . . . H32A H 0.6417 1.5959 -0.0334 0.106 Uiso 1 1 calc R . . C33 C 0.6024(5) 1.5134(5) 0.0487(4) 0.083(3) Uani 1 1 d . . . H33A H 0.5479 1.5466 0.0549 0.099 Uiso 1 1 calc R . . C34 C 0.6288(5) 1.4342(5) 0.0910(4) 0.063(2) Uani 1 1 d . . . H34A H 0.5912 1.4134 0.1259 0.076 Uiso 1 1 calc R . . C35 C 0.7101(4) 1.3849(4) 0.0824(3) 0.0457(17) Uani 1 1 d . . . H35A H 0.7269 1.3315 0.1119 0.055 Uiso 1 1 calc R . . C36 C 0.9284(4) 1.3339(4) 0.1432(3) 0.0400(16) Uani 1 1 d . . . C37 C 0.9004(4) 1.4096(4) 0.1551(3) 0.0541(19) Uani 1 1 d . . . H37A H 0.8803 1.4568 0.1195 0.065 Uiso 1 1 calc R . . C38 C 0.9015(5) 1.4170(6) 0.2175(4) 0.079(3) Uani 1 1 d . . . H38A H 0.8830 1.4690 0.2235 0.095 Uiso 1 1 calc R . . C39 C 0.9295(6) 1.3491(7) 0.2712(4) 0.080(3) Uani 1 1 d . . . H39A H 0.9303 1.3542 0.3136 0.096 Uiso 1 1 calc R . . C40 C 0.9566(5) 1.2724(6) 0.2609(3) 0.072(2) Uani 1 1 d . . . H40A H 0.9760 1.2252 0.2968 0.087 Uiso 1 1 calc R . . C41 C 0.9550(4) 1.2657(4) 0.1972(3) 0.0545(19) Uani 1 1 d . . . H41A H 0.9723 1.2136 0.1912 0.065 Uiso 1 1 calc R . . C42 C 1.1105(4) 1.2702(4) 0.0778(3) 0.0382(16) Uani 1 1 d . . . C43 C 1.1664(4) 1.2020(4) 0.0683(3) 0.0509(18) Uani 1 1 d . . . H43A H 1.1434 1.1727 0.0428 0.061 Uiso 1 1 calc R . . C44 C 1.2580(5) 1.1767(5) 0.0971(4) 0.071(2) Uani 1 1 d . . . H44A H 1.2956 1.1304 0.0909 0.085 Uiso 1 1 calc R . . C45 C 1.2914(6) 1.2200(6) 0.1339(4) 0.077(3) Uani 1 1 d . . . H45A H 1.3513 1.2018 0.1542 0.092 Uiso 1 1 calc R . . C46 C 1.2394(5) 1.2887(6) 0.1414(3) 0.067(2) Uani 1 1 d . . . H46A H 1.2645 1.3191 0.1652 0.081 Uiso 1 1 calc R . . C47 C 1.1480(4) 1.3146(4) 0.1138(3) 0.0502(18) Uani 1 1 d . . . H47A H 1.1120 1.3619 0.1197 0.060 Uiso 1 1 calc R . . C48 C 1.0590(4) 1.3061(4) -0.0755(3) 0.0385(15) Uani 1 1 d . . . C49 C 1.0365(4) 1.2683(4) -0.1223(3) 0.0469(17) Uani 1 1 d . . . H49A H 0.9786 1.2501 -0.1217 0.056 Uiso 1 1 calc R . . C50 C 1.0989(6) 1.2576(4) -0.1695(3) 0.063(2) Uani 1 1 d . . . H50A H 1.0825 1.2328 -0.2006 0.076 Uiso 1 1 calc R . . C51 C 1.1848(6) 1.2832(5) -0.1709(4) 0.073(2) Uani 1 1 d . . . H51A H 1.2276 1.2743 -0.2019 0.088 Uiso 1 1 calc R . . C52 C 1.2075(5) 1.3220(5) -0.1266(4) 0.071(2) Uani 1 1 d . . . H52A H 1.2652 1.3408 -0.1285 0.085 Uiso 1 1 calc R . . C53 C 1.1456(5) 1.3339(4) -0.0786(3) 0.0563(19) Uani 1 1 d . . . H53A H 1.1620 1.3604 -0.0487 0.068 Uiso 1 1 calc R . . C54 C 0.2772(6) 0.9138(7) 0.2122(4) 0.072(2) Uani 1 1 d . . . H54A H 0.3301 0.9366 0.2253 0.086 Uiso 1 1 calc R . . C55 C 0.2737(6) 0.8302(6) 0.2222(3) 0.071(2) Uani 1 1 d . . . H55A H 0.3236 0.7835 0.2430 0.086 Uiso 1 1 calc R . . C56 C 0.1928(6) 0.8258(6) 0.1876(4) 0.075(2) Uani 1 1 d . . . H56A H 0.1752 0.7752 0.1810 0.089 Uiso 1 1 calc R . . C57 C 0.1490(6) 0.9057(7) 0.1580(3) 0.076(3) Uani 1 1 d . . . H57A H 0.0936 0.9217 0.1274 0.091 Uiso 1 1 calc R . . C58 C 0.1990(7) 0.9599(6) 0.1735(4) 0.077(2) Uani 1 1 d . . . H58A H 0.1868 1.0209 0.1548 0.092 Uiso 1 1 calc R . . C59 C 0.2018(5) 1.0274(4) 0.3935(3) 0.0483(18) Uani 1 1 d . . . C60 C 0.2569(5) 1.0566(4) 0.4419(3) 0.069(2) Uani 1 1 d . . . H60A H 0.2449 1.1164 0.4299 0.104 Uiso 1 1 calc R . . H60B H 0.3230 1.0382 0.4400 0.104 Uiso 1 1 calc R . . H60C H 0.2374 1.0333 0.4861 0.104 Uiso 1 1 calc R . . C61 C 0.2376(5) 1.0637(4) 0.3236(3) 0.070(2) Uani 1 1 d . . . H61A H 0.2281 1.1235 0.3117 0.104 Uiso 1 1 calc R . . H61B H 0.2035 1.0469 0.2922 0.104 Uiso 1 1 calc R . . H61C H 0.3034 1.0431 0.3234 0.104 Uiso 1 1 calc R . . C62 C 0.0974(5) 1.0628(4) 0.3921(4) 0.074(2) Uani 1 1 d . . . H62A H 0.0900 1.1225 0.3815 0.111 Uiso 1 1 calc R . . H62B H 0.0729 1.0398 0.4348 0.111 Uiso 1 1 calc R . . H62C H 0.0636 1.0484 0.3592 0.111 Uiso 1 1 calc R . . C63 C 0.1484(4) 0.8575(4) 0.4790(3) 0.0428(17) Uani 1 1 d . . . C64 C 0.1766(5) 0.7638(5) 0.4864(3) 0.074(2) Uani 1 1 d . . . H64A H 0.1407 0.7316 0.5199 0.111 Uiso 1 1 calc R . . H64B H 0.2424 0.7471 0.4988 0.111 Uiso 1 1 calc R . . H64C H 0.1643 0.7543 0.4450 0.111 Uiso 1 1 calc R . . C65 C 0.0432(4) 0.8793(5) 0.4571(3) 0.065(2) Uani 1 1 d . . . H65A H 0.0071 0.8503 0.4921 0.098 Uiso 1 1 calc R . . H65B H 0.0335 0.8627 0.4184 0.098 Uiso 1 1 calc R . . H65C H 0.0235 0.9384 0.4469 0.098 Uiso 1 1 calc R . . C66 C 0.1607(5) 0.8730(5) 0.5459(3) 0.082(3) Uani 1 1 d . . . H66A H 0.1200 0.8429 0.5769 0.123 Uiso 1 1 calc R . . H66B H 0.1447 0.9316 0.5404 0.123 Uiso 1 1 calc R . . H66C H 0.2248 0.8541 0.5623 0.123 Uiso 1 1 calc R . . C67 C 0.3452(4) 0.8844(3) 0.4399(3) 0.0310(14) Uani 1 1 d . . . C68 C 0.3911(4) 0.8827(3) 0.5005(3) 0.0387(16) Uani 1 1 d . . . H68A H 0.3638 0.8692 0.5441 0.046 Uiso 1 1 calc R . . C69 C 0.4808(4) 0.9039(4) 0.4872(3) 0.0471(18) Uani 1 1 d . . . H69A H 0.5261 0.9098 0.5192 0.057 Uiso 1 1 calc R . . C70 C 0.4120(4) 0.9059(3) 0.3903(3) 0.0396(16) Uani 1 1 d . . . H70A H 0.4023 0.9115 0.3433 0.048 Uiso 1 1 calc R . . C71 C 0.4926(4) 0.9184(3) 0.4193(3) 0.0464(18) Uani 1 1 d . . . H71A H 0.5484 0.9357 0.3959 0.056 Uiso 1 1 calc R . . C72 C 0.4990(4) 0.6779(3) 0.5289(3) 0.0312(14) Uani 1 1 d . . . C73 C 0.5827(4) 0.7161(3) 0.5201(3) 0.0306(14) Uani 1 1 d . . . C74 C 0.6032(4) 0.7368(3) 0.4513(3) 0.0316(14) Uani 1 1 d . . . C75 C 0.5307(4) 0.7129(3) 0.4175(3) 0.0294(14) Uani 1 1 d . . . C76 C 0.4670(4) 0.6754(3) 0.4655(3) 0.0313(14) Uani 1 1 d . . . C77 C 0.4594(4) 0.6411(4) 0.5945(3) 0.0345(15) Uani 1 1 d . . . C78 C 0.5188(5) 0.5890(4) 0.6469(3) 0.0541(19) Uani 1 1 d . . . H78A H 0.5821 0.5751 0.6399 0.065 Uiso 1 1 calc R . . C79 C 0.4857(6) 0.5577(5) 0.7088(4) 0.075(2) Uani 1 1 d . . . H79A H 0.5271 0.5247 0.7436 0.091 Uiso 1 1 calc R . . C80 C 0.3921(7) 0.5749(5) 0.7194(4) 0.070(2) Uani 1 1 d . . . H80A H 0.3695 0.5528 0.7611 0.084 Uiso 1 1 calc R . . C81 C 0.3326(5) 0.6243(5) 0.6687(4) 0.070(2) Uani 1 1 d . . . H81A H 0.2690 0.6362 0.6758 0.084 Uiso 1 1 calc R . . C82 C 0.3657(5) 0.6572(4) 0.6067(3) 0.058(2) Uani 1 1 d . . . H82A H 0.3238 0.6910 0.5724 0.070 Uiso 1 1 calc R . . C83 C 0.6433(4) 0.7221(3) 0.5743(3) 0.0299(14) Uani 1 1 d . . . C84 C 0.7387(4) 0.6907(4) 0.5780(3) 0.0387(16) Uani 1 1 d . . . H84A H 0.7641 0.6705 0.5445 0.046 Uiso 1 1 calc R . . C85 C 0.7970(4) 0.6890(4) 0.6311(3) 0.0492(18) Uani 1 1 d . . . H85A H 0.8609 0.6685 0.6328 0.059 Uiso 1 1 calc R . . C86 C 0.7591(5) 0.7176(4) 0.6805(3) 0.0517(18) Uani 1 1 d . . . H86A H 0.7977 0.7155 0.7163 0.062 Uiso 1 1 calc R . . C87 C 0.6647(5) 0.7495(4) 0.6787(3) 0.0515(18) Uani 1 1 d . . . H87A H 0.6398 0.7688 0.7127 0.062 Uiso 1 1 calc R . . C88 C 0.6078(4) 0.7522(4) 0.6251(3) 0.0400(16) Uani 1 1 d . . . H88A H 0.5444 0.7747 0.6230 0.048 Uiso 1 1 calc R . . C89 C 0.6876(4) 0.7703(4) 0.4218(3) 0.0299(14) Uani 1 1 d . . . C90 C 0.7217(4) 0.8357(4) 0.4364(3) 0.0373(15) Uani 1 1 d . . . H90A H 0.6892 0.8609 0.4649 0.045 Uiso 1 1 calc R . . C91 C 0.8020(4) 0.8638(4) 0.4096(3) 0.0453(17) Uani 1 1 d . . . H91A H 0.8233 0.9075 0.4202 0.054 Uiso 1 1 calc R . . C92 C 0.8507(4) 0.8274(5) 0.3672(3) 0.060(2) Uani 1 1 d . . . H92A H 0.9035 0.8480 0.3475 0.072 Uiso 1 1 calc R . . C93 C 0.8215(4) 0.7606(5) 0.3541(3) 0.058(2) Uani 1 1 d . . . H93A H 0.8559 0.7343 0.3269 0.070 Uiso 1 1 calc R . . C94 C 0.7410(4) 0.7323(4) 0.3811(3) 0.0444(17) Uani 1 1 d . . . H94A H 0.7219 0.6868 0.3719 0.053 Uiso 1 1 calc R . . C95 C 0.5323(4) 0.7194(4) 0.3455(3) 0.0321(15) Uani 1 1 d . . . C96 C 0.5339(4) 0.6502(4) 0.3237(3) 0.0516(18) Uani 1 1 d . . . H96A H 0.5277 0.5989 0.3539 0.062 Uiso 1 1 calc R . . C97 C 0.5447(5) 0.6566(5) 0.2573(4) 0.068(2) Uani 1 1 d . . . H97A H 0.5469 0.6092 0.2437 0.082 Uiso 1 1 calc R . . C98 C 0.5520(5) 0.7310(6) 0.2119(4) 0.066(2) Uani 1 1 d . . . H98A H 0.5591 0.7348 0.1676 0.079 Uiso 1 1 calc R . . C99 C 0.5489(5) 0.8007(5) 0.2323(3) 0.061(2) Uani 1 1 d . . . H99A H 0.5537 0.8521 0.2017 0.073 Uiso 1 1 calc R . . C100 C 0.5388(4) 0.7941(4) 0.2982(3) 0.0437(17) Uani 1 1 d . . . H10A H 0.5363 0.8419 0.3113 0.052 Uiso 1 1 calc R . . C101 C 0.3931(4) 0.6308(4) 0.4520(3) 0.0321(14) Uani 1 1 d . . . C102 C 0.3894(4) 0.5498(4) 0.4922(3) 0.0362(15) Uani 1 1 d . . . H10B H 0.4280 0.5273 0.5305 0.043 Uiso 1 1 calc R . . C103 C 0.3289(5) 0.5028(4) 0.4755(3) 0.0512(18) Uani 1 1 d . . . H10C H 0.3268 0.4488 0.5027 0.061 Uiso 1 1 calc R . . C104 C 0.2717(4) 0.5354(5) 0.4190(4) 0.059(2) Uani 1 1 d . . . H10D H 0.2322 0.5029 0.4074 0.070 Uiso 1 1 calc R . . C105 C 0.2726(5) 0.6151(4) 0.3799(3) 0.0551(19) Uani 1 1 d . . . H10E H 0.2326 0.6374 0.3423 0.066 Uiso 1 1 calc R . . C106 C 0.3322(4) 0.6625(4) 0.3961(3) 0.0460(17) Uani 1 1 d . . . H10F H 0.3321 0.7170 0.3691 0.055 Uiso 1 1 calc R . . C200 C 1.0227(7) 0.3789(6) 0.5001(5) 0.141(4) Uani 1 1 d . . . H20A H 0.9807 0.3508 0.5310 0.212 Uiso 1 1 calc R . . H20B H 1.0580 0.4088 0.5207 0.212 Uiso 1 1 calc R . . H20C H 1.0650 0.3385 0.4863 0.212 Uiso 1 1 calc R . . C201 C 0.9677(7) 0.4383(5) 0.4416(5) 0.076(2) Uani 1 1 d . . . C203 C 0.8690(14) 0.5479(7) 0.3318(6) 0.142(6) Uani 1 1 d . . . H20H H 0.8342 0.5851 0.2952 0.170 Uiso 1 1 calc R . . C204 C 0.8236(8) 0.5023(7) 0.3820(7) 0.115(4) Uani 1 1 d . . . H20G H 0.7583 0.5085 0.3799 0.138 Uiso 1 1 calc R . . C205 C 1.0123(8) 0.4861(8) 0.3889(8) 0.131(5) Uani 1 1 d . . . H20F H 1.0775 0.4809 0.3913 0.157 Uiso 1 1 calc R . . C206 C 0.9636(13) 0.5410(9) 0.3334(8) 0.159(9) Uani 1 1 d . . . H20E H 0.9946 0.5721 0.2983 0.190 Uiso 1 1 calc R . . C207 C 0.8723(7) 0.4482(6) 0.4346(5) 0.080(3) Uani 1 1 d . . . H20D H 0.8398 0.4158 0.4679 0.096 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 Fe1 0.0287(5) 0.0376(6) 0.0305(5) -0.0085(4) 0.0018(4) -0.0050(4) Fe2 0.0272(5) 0.0332(5) 0.0328(5) -0.0112(4) 0.0030(4) -0.0085(4) Ti1 0.0383(7) 0.0548(8) 0.0339(7) -0.0134(6) 0.0099(5) -0.0114(6) Ti2 0.0332(7) 0.0529(8) 0.0322(6) -0.0171(6) 0.0008(5) -0.0046(6) Cl1 0.0707(14) 0.0758(14) 0.0778(14) -0.0245(11) 0.0265(11) -0.0371(11) Cl2 0.0609(13) 0.0598(13) 0.0786(14) -0.0191(11) 0.0171(10) -0.0016(10) Cl3 0.0520(12) 0.0744(14) 0.0557(11) -0.0170(10) -0.0086(9) 0.0128(10) Cl4 0.0490(11) 0.0665(13) 0.0705(12) -0.0283(10) 0.0051(9) -0.0185(9) P1 0.0356(10) 0.0487(11) 0.0375(10) -0.0184(9) 0.0084(8) -0.0149(8) P2 0.0270(9) 0.0433(11) 0.0334(9) -0.0174(8) 0.0008(7) -0.0029(8) N1 0.039(3) 0.044(3) 0.037(3) -0.017(3) 0.008(2) -0.005(2) N2 0.031(3) 0.034(3) 0.028(3) -0.011(2) 0.000(2) -0.001(2) C1 0.103(7) 0.099(8) 0.046(5) -0.037(5) 0.009(5) -0.038(6) C2 0.088(7) 0.135(9) 0.038(5) -0.013(6) 0.000(5) -0.064(7) C3 0.049(5) 0.142(9) 0.035(5) -0.010(6) -0.008(4) 0.000(6) C4 0.087(7) 0.084(6) 0.032(4) 0.006(4) 0.003(4) 0.007(5) C5 0.073(6) 0.104(7) 0.030(4) -0.018(5) 0.012(4) -0.017(6) C6 0.061(5) 0.039(4) 0.077(5) -0.031(4) 0.024(4) -0.020(4) C7 0.111(7) 0.081(6) 0.111(7) -0.050(5) 0.043(6) -0.058(6) C8 0.145(9) 0.031(5) 0.141(9) -0.013(5) -0.031(7) 0.005(5) C9 0.160(9) 0.072(6) 0.167(9) -0.072(7) 0.113(8) -0.052(6) C10 0.031(4) 0.081(6) 0.040(4) -0.026(4) 0.001(3) -0.016(4) C11 0.047(5) 0.124(7) 0.077(6) -0.027(5) -0.010(4) -0.018(5) C12 0.069(6) 0.142(8) 0.052(5) -0.038(5) -0.006(4) -0.007(5) C13 0.060(5) 0.069(6) 0.064(5) -0.014(4) -0.013(4) 0.003(4) C14 0.045(4) 0.037(4) 0.028(3) -0.014(3) 0.012(3) -0.018(3) C15 0.052(5) 0.038(4) 0.036(4) -0.015(3) 0.006(3) -0.010(3) C16 0.034(4) 0.046(4) 0.064(5) -0.017(4) 0.012(4) -0.006(3) C17 0.037(4) 0.043(4) 0.056(5) 0.000(4) -0.006(4) -0.006(3) C18 0.042(4) 0.041(4) 0.034(4) -0.005(3) 0.000(3) -0.011(3) C19 0.031(4) 0.041(4) 0.031(4) -0.012(3) 0.002(3) -0.009(3) C20 0.030(4) 0.034(4) 0.044(4) -0.008(3) 0.006(3) -0.006(3) C21 0.036(4) 0.033(4) 0.032(4) -0.007(3) -0.003(3) -0.007(3) C22 0.028(4) 0.046(4) 0.039(4) -0.015(3) 0.003(3) -0.011(3) C23 0.033(4) 0.037(4) 0.027(3) -0.007(3) 0.006(3) -0.007(3) C24 0.042(4) 0.029(4) 0.037(4) 0.000(3) 0.000(3) -0.001(3) C25 0.059(5) 0.076(6) 0.059(5) 0.002(4) -0.014(4) -0.024(4) C26 0.073(6) 0.088(7) 0.075(6) -0.009(5) -0.042(5) -0.013(5) C27 0.113(8) 0.083(7) 0.047(5) 0.002(5) -0.016(5) -0.007(6) C28 0.080(6) 0.073(6) 0.052(5) 0.004(5) 0.001(5) -0.011(5) C29 0.051(5) 0.051(5) 0.040(4) 0.004(4) -0.003(4) -0.010(4) C30 0.045(4) 0.035(4) 0.038(4) -0.013(3) 0.003(3) 0.000(3) C31 0.059(5) 0.047(5) 0.075(5) -0.011(4) 0.017(4) 0.009(4) C32 0.091(7) 0.060(6) 0.092(7) -0.006(5) 0.013(6) 0.023(5) C33 0.059(6) 0.080(7) 0.097(7) -0.025(6) 0.022(5) 0.024(5) C34 0.044(5) 0.076(6) 0.075(6) -0.030(5) 0.025(4) -0.010(4) C35 0.046(4) 0.042(4) 0.046(4) -0.013(3) 0.009(3) 0.000(3) C36 0.040(4) 0.047(5) 0.036(4) -0.014(4) -0.001(3) -0.014(3) C37 0.054(5) 0.060(5) 0.054(5) -0.028(4) -0.001(4) -0.004(4) C38 0.061(6) 0.116(8) 0.083(6) -0.069(6) 0.001(5) -0.002(5) C39 0.069(6) 0.130(9) 0.059(6) -0.056(6) 0.008(5) -0.016(6) C40 0.061(5) 0.109(7) 0.035(5) -0.008(5) -0.013(4) -0.007(5) C41 0.052(5) 0.064(5) 0.045(4) -0.014(4) 0.001(4) -0.007(4) C42 0.032(4) 0.043(4) 0.037(4) -0.005(3) 0.004(3) -0.011(3) C43 0.032(4) 0.053(5) 0.068(5) -0.018(4) -0.004(4) -0.007(4) C44 0.040(5) 0.077(6) 0.084(6) -0.010(5) 0.002(4) -0.004(4) C45 0.051(6) 0.103(8) 0.063(6) -0.006(5) -0.014(4) -0.009(5) C46 0.050(5) 0.101(7) 0.054(5) -0.020(5) -0.006(4) -0.028(5) C47 0.040(4) 0.067(5) 0.047(4) -0.015(4) -0.001(3) -0.023(4) C48 0.038(4) 0.036(4) 0.034(4) -0.005(3) 0.000(3) 0.002(3) C49 0.042(4) 0.052(5) 0.045(4) -0.013(4) 0.008(3) -0.006(3) C50 0.067(6) 0.070(6) 0.045(5) -0.017(4) 0.007(4) 0.011(5) C51 0.069(6) 0.098(7) 0.047(5) -0.022(5) 0.021(4) 0.004(5) C52 0.045(5) 0.096(7) 0.068(6) -0.013(5) 0.021(4) -0.022(4) C53 0.048(5) 0.067(5) 0.055(5) -0.016(4) 0.011(4) -0.016(4) C54 0.057(6) 0.117(8) 0.059(6) -0.043(6) 0.032(5) -0.037(6) C55 0.057(6) 0.099(8) 0.042(5) -0.018(5) 0.010(4) 0.034(5) C56 0.077(7) 0.110(8) 0.061(6) -0.059(6) 0.028(5) -0.023(6) C57 0.072(6) 0.115(8) 0.035(5) -0.027(5) -0.005(4) 0.008(6) C58 0.090(7) 0.078(7) 0.058(6) -0.015(5) 0.030(5) -0.013(6) C59 0.056(5) 0.040(4) 0.051(4) -0.023(4) -0.008(4) 0.004(3) C60 0.094(6) 0.042(5) 0.072(5) -0.026(4) -0.026(5) 0.005(4) C61 0.089(6) 0.043(5) 0.075(6) -0.014(4) 0.001(5) -0.011(4) C62 0.059(5) 0.063(5) 0.101(6) -0.041(5) -0.009(4) 0.024(4) C63 0.030(4) 0.072(5) 0.031(4) -0.017(4) 0.009(3) -0.017(3) C64 0.065(5) 0.076(6) 0.072(5) -0.001(5) 0.018(4) -0.029(5) C65 0.032(4) 0.110(7) 0.059(5) -0.030(5) 0.010(4) -0.020(4) C66 0.051(5) 0.166(8) 0.041(4) -0.039(5) 0.013(4) -0.037(5) C67 0.032(4) 0.031(4) 0.031(3) -0.009(3) -0.001(3) -0.009(3) C68 0.034(4) 0.040(4) 0.043(4) -0.016(3) 0.000(3) 0.000(3) C69 0.042(4) 0.037(4) 0.067(5) -0.020(4) -0.013(4) -0.011(3) C70 0.037(4) 0.038(4) 0.039(4) -0.005(3) 0.004(3) -0.003(3) C71 0.031(4) 0.030(4) 0.069(5) 0.000(4) 0.011(4) -0.006(3) C72 0.031(4) 0.032(4) 0.033(4) -0.013(3) 0.003(3) -0.006(3) C73 0.032(4) 0.028(4) 0.034(4) -0.011(3) 0.004(3) -0.006(3) C74 0.027(3) 0.035(4) 0.037(4) -0.015(3) 0.001(3) -0.010(3) C75 0.029(3) 0.025(3) 0.035(4) -0.009(3) 0.001(3) -0.008(3) C76 0.025(3) 0.035(4) 0.031(3) -0.005(3) -0.002(3) -0.005(3) C77 0.035(4) 0.039(4) 0.034(4) -0.011(3) 0.003(3) -0.020(3) C78 0.042(4) 0.064(5) 0.046(4) 0.001(4) -0.001(4) -0.017(4) C79 0.079(6) 0.082(6) 0.048(5) 0.016(4) -0.006(5) -0.033(5) C80 0.097(7) 0.079(6) 0.039(5) -0.012(4) 0.021(5) -0.040(5) C81 0.063(5) 0.094(7) 0.062(5) -0.031(5) 0.031(5) -0.026(5) C82 0.041(5) 0.086(6) 0.044(4) -0.012(4) 0.014(4) -0.015(4) C83 0.027(4) 0.031(4) 0.032(3) -0.010(3) 0.002(3) -0.003(3) C84 0.039(4) 0.043(4) 0.036(4) -0.013(3) -0.006(3) -0.007(3) C85 0.032(4) 0.057(5) 0.054(5) -0.011(4) -0.009(3) -0.007(3) C86 0.058(5) 0.061(5) 0.036(4) -0.013(4) -0.009(4) -0.012(4) C87 0.061(5) 0.064(5) 0.040(4) -0.025(4) 0.007(4) -0.023(4) C88 0.031(4) 0.053(4) 0.038(4) -0.017(3) 0.002(3) -0.007(3) C89 0.023(3) 0.035(4) 0.029(3) -0.007(3) -0.002(3) -0.002(3) C90 0.032(4) 0.041(4) 0.040(4) -0.013(3) -0.002(3) -0.006(3) C91 0.037(4) 0.049(4) 0.056(4) -0.017(4) 0.002(3) -0.021(3) C92 0.035(4) 0.091(6) 0.066(5) -0.032(5) 0.024(4) -0.027(4) C93 0.032(4) 0.094(6) 0.062(5) -0.043(5) 0.015(4) -0.012(4) C94 0.031(4) 0.057(5) 0.055(4) -0.029(4) 0.007(3) -0.014(3) C95 0.028(3) 0.041(4) 0.032(4) -0.012(3) 0.005(3) -0.015(3) C96 0.068(5) 0.047(5) 0.043(4) -0.016(4) 0.007(4) -0.015(4) C97 0.083(6) 0.080(6) 0.056(5) -0.042(5) 0.002(4) -0.013(5) C98 0.066(5) 0.099(7) 0.034(4) -0.022(5) 0.007(4) -0.014(5) C99 0.064(5) 0.068(6) 0.038(5) 0.000(4) 0.007(4) -0.011(4) C100 0.042(4) 0.049(5) 0.041(4) -0.016(4) 0.011(3) -0.008(3) C101 0.033(4) 0.029(4) 0.037(4) -0.012(3) 0.003(3) -0.006(3) C102 0.028(4) 0.030(4) 0.052(4) -0.014(3) 0.004(3) -0.004(3) C103 0.049(5) 0.037(4) 0.068(5) -0.011(4) 0.008(4) -0.017(4) C104 0.032(4) 0.064(6) 0.094(6) -0.040(5) -0.007(4) -0.017(4) C105 0.052(5) 0.048(5) 0.067(5) -0.021(4) -0.013(4) -0.007(4) C106 0.049(4) 0.041(4) 0.053(4) -0.021(4) -0.002(4) -0.010(3) C200 0.153(11) 0.121(10) 0.148(10) -0.059(8) -0.044(9) 0.020(8) C201 0.079(7) 0.065(6) 0.098(7) -0.043(6) 0.017(6) -0.016(6) C203 0.29(2) 0.067(8) 0.071(8) -0.031(6) 0.037(11) -0.018(12) C204 0.122(10) 0.067(8) 0.161(12) -0.049(8) -0.027(10) 0.000(7) C205 0.095(9) 0.093(10) 0.237(16) -0.086(10) 0.082(11) -0.045(8) C206 0.24(2) 0.086(10) 0.178(15) -0.068(10) 0.167(16) -0.056(13) C207 0.074(7) 0.063(6) 0.114(8) -0.039(6) 0.030(6) -0.020(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 Fe1 C16 2.031(6) . ? Fe1 C17 2.047(6) . ? Fe1 C22 2.062(6) . ? Fe1 C23 2.068(5) . ? Fe1 C18 2.074(6) . ? Fe1 C15 2.080(6) . ? Fe1 C19 2.081(6) . ? Fe1 C21 2.081(6) . ? Fe1 C20 2.095(6) . ? Fe1 C14 2.142(5) . ? Fe2 C69 2.029(6) . ? Fe2 C71 2.029(6) . ? Fe2 C75 2.050(5) . ? Fe2 C74 2.061(5) . ? Fe2 C68 2.065(6) . ? Fe2 C73 2.067(6) . ? Fe2 C70 2.068(6) . ? Fe2 C72 2.087(6) . ? Fe2 C76 2.089(6) . ? Fe2 C67 2.122(6) . ? Ti1 N1 1.755(4) . ? Ti1 Cl2 2.286(2) . ? Ti1 Cl1 2.317(2) . ? Ti1 C2 2.339(8) . ? Ti1 C3 2.352(7) . ? Ti1 C4 2.359(7) . ? Ti1 C1 2.404(7) . ? Ti1 C5 2.407(6) . ? Ti2 N2 1.769(4) . ? Ti2 Cl4 2.290(2) . ? Ti2 Cl3 2.312(2) . ? Ti2 C55 2.352(6) . ? Ti2 C54 2.354(7) . ? Ti2 C58 2.366(7) . ? Ti2 C56 2.385(7) . ? Ti2 C57 2.399(7) . ? P1 N1 1.606(4) . ? P1 C14 1.807(6) . ? P1 C10 1.851(6) . ? P1 C6 1.878(6) . ? P2 N2 1.600(4) . ? P2 C67 1.810(6) . ? P2 C63 1.838(6) . ? P2 C59 1.867(6) . ? C1 C5 1.370(10) . ? C1 C2 1.418(10) . ? C2 C3 1.384(11) . ? C3 C4 1.391(10) . ? C4 C5 1.383(9) . ? C6 C9 1.515(9) . ? C6 C7 1.516(9) . ? C6 C8 1.538(10) . ? C10 C13 1.511(8) . ? C10 C12 1.536(8) . ? C10 C11 1.547(8) . ? C14 C15 1.430(7) . ? C14 C18 1.442(7) . ? C15 C16 1.410(8) . ? C16 C17 1.414(8) . ? C17 C18 1.405(8) . ? C19 C20 1.431(7) . ? C19 C23 1.432(7) . ? C19 C24 1.488(7) . ? C20 C21 1.442(7) . ? C20 C30 1.487(8) . ? C21 C22 1.438(7) . ? C21 C36 1.466(8) . ? C22 C23 1.440(7) . ? C22 C42 1.495(8) . ? C23 C48 1.480(7) . ? C24 C25 1.369(8) . ? C24 C29 1.382(7) . ? C25 C26 1.399(9) . ? C26 C27 1.368(10) . ? C27 C28 1.345(10) . ? C28 C29 1.380(8) . ? C30 C31 1.385(8) . ? C30 C35 1.386(8) . ? C31 C32 1.370(9) . ? C32 C33 1.389(10) . ? C33 C34 1.370(9) . ? C34 C35 1.380(8) . ? C36 C41 1.367(8) . ? C36 C37 1.386(8) . ? C37 C38 1.367(9) . ? C38 C39 1.362(10) . ? C39 C40 1.386(10) . ? C40 C41 1.389(9) . ? C42 C43 1.375(8) . ? C42 C47 1.383(8) . ? C43 C44 1.402(8) . ? C44 C45 1.354(10) . ? C45 C46 1.342(10) . ? C46 C47 1.393(9) . ? C48 C53 1.393(8) . ? C48 C49 1.397(8) . ? C49 C50 1.378(8) . ? C50 C51 1.369(9) . ? C51 C52 1.364(9) . ? C52 C53 1.392(9) . ? C54 C58 1.380(10) . ? C54 C55 1.382(10) . ? C55 C56 1.400(10) . ? C56 C57 1.366(10) . ? C57 C58 1.362(10) . ? C59 C62 1.530(8) . ? C59 C60 1.535(8) . ? C59 C61 1.544(8) . ? C63 C66 1.532(8) . ? C63 C65 1.542(8) . ? C63 C64 1.544(8) . ? C67 C70 1.426(7) . ? C67 C68 1.436(7) . ? C68 C69 1.397(7) . ? C69 C71 1.399(8) . ? C70 C71 1.387(8) . ? C72 C76 1.436(7) . ? C72 C73 1.438(7) . ? C72 C77 1.494(7) . ? C73 C74 1.434(7) . ? C73 C83 1.479(7) . ? C74 C75 1.439(7) . ? C74 C89 1.477(7) . ? C75 C76 1.437(7) . ? C75 C95 1.497(7) . ? C76 C101 1.470(7) . ? C77 C82 1.376(8) . ? C77 C78 1.389(8) . ? C78 C79 1.372(8) . ? C79 C80 1.369(9) . ? C80 C81 1.356(9) . ? C81 C82 1.379(8) . ? C83 C84 1.390(7) . ? C83 C88 1.391(7) . ? C84 C85 1.395(7) . ? C85 C86 1.362(8) . ? C86 C87 1.382(8) . ? C87 C88 1.387(7) . ? C89 C94 1.393(7) . ? C89 C90 1.393(7) . ? C90 C91 1.373(7) . ? C91 C92 1.374(8) . ? C92 C93 1.371(8) . ? C93 C94 1.379(8) . ? C95 C100 1.376(7) . ? C95 C96 1.383(7) . ? C96 C97 1.389(8) . ? C97 C98 1.358(9) . ? C98 C99 1.371(9) . ? C99 C100 1.378(8) . ? C101 C102 1.391(7) . ? C101 C106 1.393(7) . ? C102 C103 1.379(8) . ? C103 C104 1.372(8) . ? C104 C105 1.359(8) . ? C105 C106 1.370(8) . ? C200 C201 1.479(11) . ? C201 C207 1.360(11) . ? C201 C205 1.389(13) . ? C203 C204 1.345(14) . ? C203 C206 1.349(18) . ? C204 C207 1.330(12) . ? C205 C206 1.375(17) . ? 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 C16 Fe1 C17 40.6(2) . . ? C16 Fe1 C22 110.2(2) . . ? C17 Fe1 C22 98.6(2) . . ? C16 Fe1 C23 101.3(2) . . ? C17 Fe1 C23 118.4(2) . . ? C22 Fe1 C23 40.8(2) . . ? C16 Fe1 C18 67.0(2) . . ? C17 Fe1 C18 39.9(2) . . ? C22 Fe1 C18 122.3(2) . . ? C23 Fe1 C18 156.8(2) . . ? C16 Fe1 C15 40.1(2) . . ? C17 Fe1 C15 68.0(2) . . ? C22 Fe1 C15 146.7(2) . . ? C23 Fe1 C15 117.5(2) . . ? C18 Fe1 C15 67.2(2) . . ? C16 Fe1 C19 125.7(2) . . ? C17 Fe1 C19 158.1(2) . . ? C22 Fe1 C19 68.2(2) . . ? C23 Fe1 C19 40.4(2) . . ? C18 Fe1 C19 162.0(2) . . ? C15 Fe1 C19 113.0(2) . . ? C16 Fe1 C21 145.4(2) . . ? C17 Fe1 C21 113.6(2) . . ? C22 Fe1 C21 40.6(2) . . ? C23 Fe1 C21 68.5(2) . . ? C18 Fe1 C21 109.1(2) . . ? C15 Fe1 C21 172.7(2) . . ? C19 Fe1 C21 68.4(2) . . ? C16 Fe1 C20 165.8(2) . . ? C17 Fe1 C20 152.1(3) . . ? C22 Fe1 C20 67.6(2) . . ? C23 Fe1 C20 67.5(2) . . ? C18 Fe1 C20 126.6(2) . . ? C15 Fe1 C20 136.2(2) . . ? C19 Fe1 C20 40.1(2) . . ? C21 Fe1 C20 40.4(2) . . ? C16 Fe1 C14 66.6(2) . . ? C17 Fe1 C14 67.2(2) . . ? C22 Fe1 C14 162.2(2) . . ? C23 Fe1 C14 155.3(2) . . ? C18 Fe1 C14 40.0(2) . . ? C15 Fe1 C14 39.6(2) . . ? C19 Fe1 C14 128.6(2) . . ? C21 Fe1 C14 133.7(2) . . ? C20 Fe1 C14 120.0(2) . . ? C69 Fe2 C71 40.3(2) . . ? C69 Fe2 C75 148.7(2) . . ? C71 Fe2 C75 116.3(2) . . ? C69 Fe2 C74 112.4(2) . . ? C71 Fe2 C74 99.8(2) . . ? C75 Fe2 C74 40.99(19) . . ? C69 Fe2 C68 39.9(2) . . ? C71 Fe2 C68 66.9(2) . . ? C75 Fe2 C68 169.4(2) . . ? C74 Fe2 C68 149.6(2) . . ? C69 Fe2 C73 101.7(2) . . ? C71 Fe2 C73 117.9(2) . . ? C75 Fe2 C73 68.6(2) . . ? C74 Fe2 C73 40.7(2) . . ? C68 Fe2 C73 119.7(2) . . ? C69 Fe2 C70 67.2(2) . . ? C71 Fe2 C70 39.5(2) . . ? C75 Fe2 C70 108.7(2) . . ? C74 Fe2 C70 121.0(2) . . ? C68 Fe2 C70 66.8(2) . . ? C73 Fe2 C70 155.2(2) . . ? C69 Fe2 C72 124.3(2) . . ? C71 Fe2 C72 157.0(2) . . ? C75 Fe2 C72 68.1(2) . . ? C74 Fe2 C72 68.2(2) . . ? C68 Fe2 C72 113.2(2) . . ? C73 Fe2 C72 40.5(2) . . ? C70 Fe2 C72 163.4(2) . . ? C69 Fe2 C76 164.2(2) . . ? C71 Fe2 C76 155.0(2) . . ? C75 Fe2 C76 40.61(19) . . ? C74 Fe2 C76 68.4(2) . . ? C68 Fe2 C76 133.6(2) . . ? C73 Fe2 C76 68.2(2) . . ? C70 Fe2 C76 126.9(2) . . ? C72 Fe2 C76 40.23(19) . . ? C69 Fe2 C67 67.4(2) . . ? C71 Fe2 C67 66.9(2) . . ? C75 Fe2 C67 130.5(2) . . ? C74 Fe2 C67 160.4(2) . . ? C68 Fe2 C67 40.08(19) . . ? C73 Fe2 C67 158.1(2) . . ? C70 Fe2 C67 39.8(2) . . ? C72 Fe2 C67 129.3(2) . . ? C76 Fe2 C67 117.5(2) . . ? N1 Ti1 Cl2 103.25(16) . . ? N1 Ti1 Cl1 103.17(16) . . ? Cl2 Ti1 Cl1 101.12(8) . . ? N1 Ti1 C2 102.9(3) . . ? Cl2 Ti1 C2 99.0(3) . . ? Cl1 Ti1 C2 142.2(2) . . ? N1 Ti1 C3 93.5(3) . . ? Cl2 Ti1 C3 133.2(3) . . ? Cl1 Ti1 C3 117.2(3) . . ? C2 Ti1 C3 34.3(3) . . ? N1 Ti1 C4 116.8(3) . . ? Cl2 Ti1 C4 136.5(2) . . ? Cl1 Ti1 C4 86.3(2) . . ? C2 Ti1 C4 57.4(3) . . ? C3 Ti1 C4 34.3(2) . . ? N1 Ti1 C1 136.9(3) . . ? Cl2 Ti1 C1 83.1(2) . . ? Cl1 Ti1 C1 117.5(2) . . ? C2 Ti1 C1 34.8(3) . . ? C3 Ti1 C1 56.5(3) . . ? C4 Ti1 C1 56.3(3) . . ? N1 Ti1 C5 148.8(3) . . ? Cl2 Ti1 C5 103.2(2) . . ? Cl1 Ti1 C5 87.7(2) . . ? C2 Ti1 C5 56.5(3) . . ? C3 Ti1 C5 55.9(3) . . ? C4 Ti1 C5 33.7(2) . . ? C1 Ti1 C5 33.1(2) . . ? N2 Ti2 Cl4 104.00(15) . . ? N2 Ti2 Cl3 103.02(15) . . ? Cl4 Ti2 Cl3 99.79(8) . . ? N2 Ti2 C55 103.0(3) . . ? Cl4 Ti2 C55 100.4(3) . . ? Cl3 Ti2 C55 141.9(2) . . ? N2 Ti2 C54 93.5(2) . . ? Cl4 Ti2 C54 134.4(3) . . ? Cl3 Ti2 C54 117.0(3) . . ? C55 Ti2 C54 34.2(2) . . ? N2 Ti2 C58 117.0(3) . . ? Cl4 Ti2 C58 135.8(3) . . ? Cl3 Ti2 C58 86.8(2) . . ? C55 Ti2 C58 56.6(3) . . ? C54 Ti2 C58 34.0(2) . . ? N2 Ti2 C56 136.5(3) . . ? Cl4 Ti2 C56 83.6(2) . . ? Cl3 Ti2 C56 118.0(3) . . ? C55 Ti2 C56 34.4(2) . . ? C54 Ti2 C56 56.4(3) . . ? C58 Ti2 C56 55.8(3) . . ? N2 Ti2 C57 148.5(3) . . ? Cl4 Ti2 C57 102.9(3) . . ? Cl3 Ti2 C57 88.1(2) . . ? C55 Ti2 C57 56.0(3) . . ? C54 Ti2 C57 55.6(3) . . ? C58 Ti2 C57 33.2(2) . . ? C56 Ti2 C57 33.2(2) . . ? N1 P1 C14 111.5(3) . . ? N1 P1 C10 107.9(3) . . ? C14 P1 C10 111.7(3) . . ? N1 P1 C6 108.5(3) . . ? C14 P1 C6 102.6(3) . . ? C10 P1 C6 114.6(3) . . ? N2 P2 C67 112.8(2) . . ? N2 P2 C63 107.4(3) . . ? C67 P2 C63 111.4(3) . . ? N2 P2 C59 108.6(3) . . ? C67 P2 C59 102.2(3) . . ? C63 P2 C59 114.5(3) . . ? P1 N1 Ti1 170.0(3) . . ? P2 N2 Ti2 164.1(3) . . ? C5 C1 C2 107.4(8) . . ? C5 C1 Ti1 73.6(4) . . ? C2 C1 Ti1 70.1(4) . . ? C3 C2 C1 106.9(8) . . ? C3 C2 Ti1 73.4(5) . . ? C1 C2 Ti1 75.1(4) . . ? C2 C3 C4 108.9(8) . . ? C2 C3 Ti1 72.3(5) . . ? C4 C3 Ti1 73.1(4) . . ? C5 C4 C3 107.1(8) . . ? C5 C4 Ti1 75.0(4) . . ? C3 C4 Ti1 72.6(4) . . ? C1 C5 C4 109.5(8) . . ? C1 C5 Ti1 73.3(4) . . ? C4 C5 Ti1 71.2(4) . . ? C9 C6 C7 108.1(6) . . ? C9 C6 C8 109.9(7) . . ? C7 C6 C8 107.0(6) . . ? C9 C6 P1 114.1(5) . . ? C7 C6 P1 111.4(5) . . ? C8 C6 P1 106.1(5) . . ? C13 C10 C12 110.8(6) . . ? C13 C10 C11 106.8(6) . . ? C12 C10 C11 110.0(5) . . ? C13 C10 P1 105.3(4) . . ? C12 C10 P1 112.5(5) . . ? C11 C10 P1 111.3(5) . . ? C15 C14 C18 106.4(5) . . ? C15 C14 P1 128.9(4) . . ? C18 C14 P1 118.0(4) . . ? C15 C14 Fe1 67.9(3) . . ? C18 C14 Fe1 67.5(3) . . ? P1 C14 Fe1 151.8(3) . . ? C16 C15 C14 107.7(5) . . ? C16 C15 Fe1 68.1(3) . . ? C14 C15 Fe1 72.5(3) . . ? C15 C16 C17 109.7(6) . . ? C15 C16 Fe1 71.8(3) . . ? C17 C16 Fe1 70.3(4) . . ? C18 C17 C16 107.0(6) . . ? C18 C17 Fe1 71.1(3) . . ? C16 C17 Fe1 69.1(4) . . ? C17 C18 C14 109.2(5) . . ? C17 C18 Fe1 69.0(3) . . ? C14 C18 Fe1 72.6(3) . . ? C20 C19 C23 107.7(5) . . ? C20 C19 C24 127.2(5) . . ? C23 C19 C24 124.0(5) . . ? C20 C19 Fe1 70.5(3) . . ? C23 C19 Fe1 69.4(3) . . ? C24 C19 Fe1 134.8(4) . . ? C19 C20 C21 109.0(5) . . ? C19 C20 C30 126.0(5) . . ? C21 C20 C30 124.4(5) . . ? C19 C20 Fe1 69.4(3) . . ? C21 C20 Fe1 69.3(3) . . ? C30 C20 Fe1 134.6(4) . . ? C22 C21 C20 106.8(5) . . ? C22 C21 C36 125.6(5) . . ? C20 C21 C36 127.1(5) . . ? C22 C21 Fe1 69.0(3) . . ? C20 C21 Fe1 70.3(3) . . ? C36 C21 Fe1 131.9(4) . . ? C21 C22 C23 108.5(5) . . ? C21 C22 C42 125.7(5) . . ? C23 C22 C42 125.5(5) . . ? C21 C22 Fe1 70.4(3) . . ? C23 C22 Fe1 69.8(3) . . ? C42 C22 Fe1 130.0(4) . . ? C19 C23 C22 108.0(5) . . ? C19 C23 C48 125.4(5) . . ? C22 C23 C48 126.5(5) . . ? C19 C23 Fe1 70.3(3) . . ? C22 C23 Fe1 69.4(3) . . ? C48 C23 Fe1 129.9(4) . . ? C25 C24 C29 117.5(6) . . ? C25 C24 C19 123.9(6) . . ? C29 C24 C19 118.6(6) . . ? C24 C25 C26 120.8(7) . . ? C27 C26 C25 120.0(7) . . ? C28 C27 C26 119.8(8) . . ? C27 C28 C29 120.4(8) . . ? C28 C29 C24 121.5(7) . . ? C31 C30 C35 117.4(6) . . ? C31 C30 C20 119.7(6) . . ? C35 C30 C20 122.6(6) . . ? C32 C31 C30 121.6(7) . . ? C31 C32 C33 120.4(8) . . ? C34 C33 C32 118.4(7) . . ? C33 C34 C35 121.0(7) . . ? C34 C35 C30 121.0(6) . . ? C41 C36 C37 116.8(6) . . ? C41 C36 C21 123.4(6) . . ? C37 C36 C21 119.7(6) . . ? C38 C37 C36 122.2(7) . . ? C39 C38 C37 120.7(8) . . ? C38 C39 C40 118.4(8) . . ? C39 C40 C41 120.2(7) . . ? C36 C41 C40 121.6(7) . . ? C43 C42 C47 118.5(6) . . ? C43 C42 C22 122.0(6) . . ? C47 C42 C22 119.1(6) . . ? C42 C43 C44 120.2(7) . . ? C45 C44 C43 119.7(8) . . ? C46 C45 C44 121.0(8) . . ? C45 C46 C47 120.2(7) . . ? C42 C47 C46 120.2(7) . . ? C53 C48 C49 118.0(6) . . ? C53 C48 C23 120.1(6) . . ? C49 C48 C23 121.9(6) . . ? C50 C49 C48 121.0(6) . . ? C51 C50 C49 120.4(7) . . ? C52 C51 C50 119.6(7) . . ? C51 C52 C53 121.1(7) . . ? C52 C53 C48 119.9(7) . . ? C58 C54 C55 108.1(8) . . ? C58 C54 Ti2 73.5(4) . . ? C55 C54 Ti2 72.9(4) . . ? C54 C55 C56 107.1(7) . . ? C54 C55 Ti2 73.0(4) . . ? C56 C55 Ti2 74.1(4) . . ? C57 C56 C55 107.6(8) . . ? C57 C56 Ti2 74.0(4) . . ? C55 C56 Ti2 71.5(4) . . ? C58 C57 C56 109.2(8) . . ? C58 C57 Ti2 72.1(4) . . ? C56 C57 Ti2 72.8(4) . . ? C57 C58 C54 108.0(8) . . ? C57 C58 Ti2 74.7(5) . . ? C54 C58 Ti2 72.5(4) . . ? C62 C59 C60 109.5(5) . . ? C62 C59 C61 107.9(6) . . ? C60 C59 C61 107.8(6) . . ? C62 C59 P2 112.0(5) . . ? C60 C59 P2 111.8(4) . . ? C61 C59 P2 107.7(4) . . ? C66 C63 C65 108.8(5) . . ? C66 C63 C64 110.3(6) . . ? C65 C63 C64 105.9(5) . . ? C66 C63 P2 114.9(4) . . ? C65 C63 P2 111.7(4) . . ? C64 C63 P2 104.9(4) . . ? C70 C67 C68 105.4(5) . . ? C70 C67 P2 117.7(4) . . ? C68 C67 P2 129.8(4) . . ? C70 C67 Fe2 68.1(3) . . ? C68 C67 Fe2 67.8(3) . . ? P2 C67 Fe2 151.2(3) . . ? C69 C68 C67 108.9(5) . . ? C69 C68 Fe2 68.6(3) . . ? C67 C68 Fe2 72.1(3) . . ? C68 C69 C71 107.7(6) . . ? C68 C69 Fe2 71.5(3) . . ? C71 C69 Fe2 69.9(4) . . ? C71 C70 C67 108.9(5) . . ? C71 C70 Fe2 68.7(3) . . ? C67 C70 Fe2 72.2(3) . . ? C70 C71 C69 109.1(6) . . ? C70 C71 Fe2 71.8(3) . . ? C69 C71 Fe2 69.8(3) . . ? C76 C72 C73 108.3(5) . . ? C76 C72 C77 127.2(5) . . ? C73 C72 C77 124.3(5) . . ? C76 C72 Fe2 70.0(3) . . ? C73 C72 Fe2 69.0(3) . . ? C77 C72 Fe2 130.8(4) . . ? C74 C73 C72 108.1(5) . . ? C74 C73 C83 126.3(5) . . ? C72 C73 C83 125.2(5) . . ? C74 C73 Fe2 69.5(3) . . ? C72 C73 Fe2 70.5(3) . . ? C83 C73 Fe2 131.7(4) . . ? C73 C74 C75 107.7(5) . . ? C73 C74 C89 125.9(5) . . ? C75 C74 C89 126.3(5) . . ? C73 C74 Fe2 69.9(3) . . ? C75 C74 Fe2 69.1(3) . . ? C89 C74 Fe2 130.0(4) . . ? C76 C75 C74 108.5(5) . . ? C76 C75 C95 128.3(5) . . ? C74 C75 C95 122.9(5) . . ? C76 C75 Fe2 71.2(3) . . ? C74 C75 Fe2 69.9(3) . . ? C95 C75 Fe2 129.7(4) . . ? C72 C76 C75 107.5(5) . . ? C72 C76 C101 127.2(5) . . ? C75 C76 C101 124.5(5) . . ? C72 C76 Fe2 69.8(3) . . ? C75 C76 Fe2 68.2(3) . . ? C101 C76 Fe2 134.9(4) . . ? C82 C77 C78 117.2(6) . . ? C82 C77 C72 123.1(6) . . ? C78 C77 C72 119.7(5) . . ? C79 C78 C77 121.2(7) . . ? C80 C79 C78 120.2(7) . . ? C81 C80 C79 119.5(7) . . ? C80 C81 C82 120.5(7) . . ? C77 C82 C81 121.2(7) . . ? C84 C83 C88 117.8(5) . . ? C84 C83 C73 119.3(5) . . ? C88 C83 C73 122.8(5) . . ? C83 C84 C85 121.3(6) . . ? C86 C85 C84 119.1(6) . . ? C85 C86 C87 121.6(6) . . ? C86 C87 C88 118.7(6) . . ? C87 C88 C83 121.5(6) . . ? C94 C89 C90 116.9(5) . . ? C94 C89 C74 119.9(5) . . ? C90 C89 C74 123.1(5) . . ? C91 C90 C89 121.7(6) . . ? C90 C91 C92 120.0(6) . . ? C93 C92 C91 119.8(6) . . ? C92 C93 C94 120.1(6) . . ? C93 C94 C89 121.4(6) . . ? C100 C95 C96 117.0(5) . . ? C100 C95 C75 120.9(5) . . ? C96 C95 C75 122.0(5) . . ? C95 C96 C97 120.7(6) . . ? C98 C97 C96 120.9(7) . . ? C97 C98 C99 119.3(7) . . ? C98 C99 C100 119.7(7) . . ? C95 C100 C99 122.4(6) . . ? C102 C101 C106 117.6(5) . . ? C102 C101 C76 119.5(5) . . ? C106 C101 C76 122.5(5) . . ? C103 C102 C101 120.5(6) . . ? C104 C103 C102 120.2(6) . . ? C105 C104 C103 120.3(6) . . ? C104 C105 C106 120.0(7) . . ? C105 C106 C101 121.4(6) . . ? C207 C201 C205 115.7(10) . . ? C207 C201 C200 123.4(10) . . ? C205 C201 C200 120.8(11) . . ? C204 C203 C206 121.7(15) . . ? C207 C204 C203 120.0(13) . . ? C206 C205 C201 122.5(13) . . ? C203 C206 C205 117.3(14) . . ? C204 C207 C201 122.8(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.362 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.068 #===end data_[Fe{5-C5H4PtBu2(NSiMe3)}2] _database_code_depnum_ccdc_archive 'CCDC 747511' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C32 H72 Fe N2 P2 Si2' _chemical_formula_weight 658.89 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 26.915(3) _cell_length_b 9.7197(11) _cell_length_c 15.1251(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.8850(10) _cell_angle_gamma 90.00 _cell_volume 3824.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.495593 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 298(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 17871 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3370 _reflns_number_gt 2817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 Rfactors 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^)+(0.0611P)^2^+1.3658P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 3370 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Fe1 Fe 0.0000 0.77663(4) 0.2500 0.04281(14) Uani 1 2 d S . . P1 P -0.125066(19) 0.85071(5) 0.27408(4) 0.04253(16) Uani 1 1 d . . . N1 N -0.11803(8) 0.7612(2) 0.35910(13) 0.0603(5) Uani 1 1 d . . . Si1 Si -0.11931(3) 0.65817(6) 0.44491(4) 0.05396(18) Uani 1 1 d . . . C1 C -0.07800(7) 0.8104(2) 0.21158(13) 0.0435(4) Uani 1 1 d . . . C2 C -0.05273(7) 0.8921(2) 0.15734(13) 0.0493(5) Uani 1 1 d . . . H2A H -0.0533 0.9928 0.1534 0.059 Uiso 1 1 calc R . . C3 C -0.02610(9) 0.8028(3) 0.11141(15) 0.0620(6) Uani 1 1 d . . . H3A H -0.0053 0.8311 0.0701 0.074 Uiso 1 1 calc R . . C4 C -0.03395(9) 0.6678(3) 0.13604(18) 0.0678(7) Uani 1 1 d . . . H4A H -0.0199 0.5851 0.1143 0.081 Uiso 1 1 calc R . . C5 C -0.06543(8) 0.6703(2) 0.19768(17) 0.0559(6) Uani 1 1 d . . . H5A H -0.0771 0.5896 0.2256 0.067 Uiso 1 1 calc R . . C6 C -0.12012(8) 1.0373(2) 0.30537(16) 0.0539(5) Uani 1 1 d . . . C7 C -0.06377(10) 1.0688(3) 0.3526(2) 0.0745(7) Uani 1 1 d . . . H7A H -0.0603 1.1642 0.3693 0.112 Uiso 1 1 calc R . . H7B H -0.0428 1.0487 0.3116 0.112 Uiso 1 1 calc R . . H7C H -0.0529 1.0131 0.4066 0.112 Uiso 1 1 calc R . . C8 C -0.15083(12) 1.0619(3) 0.3766(2) 0.0799(8) Uani 1 1 d . . . H8A H -0.1487 1.1573 0.3936 0.120 Uiso 1 1 calc R . . H8B H -0.1368 1.0065 0.4297 0.120 Uiso 1 1 calc R . . H8C H -0.1861 1.0373 0.3509 0.120 Uiso 1 1 calc R . . C9 C -0.13895(12) 1.1372(3) 0.2250(2) 0.0780(8) Uani 1 1 d . . . H9A H -0.1350 1.2302 0.2472 0.117 Uiso 1 1 calc R . . H9B H -0.1745 1.1197 0.1963 0.117 Uiso 1 1 calc R . . H9C H -0.1191 1.1243 0.1813 0.117 Uiso 1 1 calc R . . C10 C -0.18672(8) 0.8130(3) 0.18576(17) 0.0596(6) Uani 1 1 d . . . C11 C -0.18797(11) 0.8708(4) 0.09111(18) 0.0882(9) Uani 1 1 d . . . H11A H -0.2203 0.8483 0.0492 0.132 Uiso 1 1 calc R . . H11B H -0.1604 0.8313 0.0699 0.132 Uiso 1 1 calc R . . H11C H -0.1840 0.9689 0.0949 0.132 Uiso 1 1 calc R . . C12 C -0.19108(10) 0.6554(3) 0.1781(2) 0.0828(8) Uani 1 1 d . . . H12A H -0.2222 0.6311 0.1336 0.124 Uiso 1 1 calc R . . H12B H -0.1916 0.6173 0.2364 0.124 Uiso 1 1 calc R . . H12C H -0.1621 0.6193 0.1595 0.124 Uiso 1 1 calc R . . C13 C -0.23291(9) 0.8653(4) 0.2180(2) 0.0892(9) Uani 1 1 d . . . H13A H -0.2641 0.8452 0.1723 0.134 Uiso 1 1 calc R . . H13B H -0.2299 0.9629 0.2277 0.134 Uiso 1 1 calc R . . H13C H -0.2336 0.8204 0.2743 0.134 Uiso 1 1 calc R . . C14 C -0.11061(15) 0.4740(3) 0.4161(2) 0.0987(11) Uani 1 1 d . . . H14A H -0.1376 0.4476 0.3640 0.148 Uiso 1 1 calc R . . H14B H -0.1118 0.4169 0.4673 0.148 Uiso 1 1 calc R . . H14C H -0.0780 0.4631 0.4022 0.148 Uiso 1 1 calc R . . C15 C -0.18118(13) 0.6717(4) 0.4788(2) 0.1029(11) Uani 1 1 d . . . H15A H -0.2092 0.6487 0.4275 0.154 Uiso 1 1 calc R . . H15B H -0.1854 0.7641 0.4981 0.154 Uiso 1 1 calc R . . H15C H -0.1807 0.6093 0.5282 0.154 Uiso 1 1 calc R . . C16 C -0.06577(12) 0.7020(3) 0.54710(17) 0.0768(8) Uani 1 1 d . . . H16A H -0.0335 0.6948 0.5314 0.115 Uiso 1 1 calc R . . H16B H -0.0661 0.6393 0.5960 0.115 Uiso 1 1 calc R . . H16C H -0.0702 0.7943 0.5663 0.115 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 Fe1 0.0346(2) 0.0457(2) 0.0486(2) 0.000 0.01157(17) 0.000 P1 0.0353(3) 0.0473(3) 0.0451(3) 0.0010(2) 0.0105(2) 0.0007(2) N1 0.0656(12) 0.0595(11) 0.0583(12) 0.0087(9) 0.0204(10) 0.0029(10) Si1 0.0655(4) 0.0472(3) 0.0493(4) 0.0016(3) 0.0150(3) -0.0063(3) C1 0.0318(9) 0.0519(11) 0.0452(11) -0.0043(9) 0.0072(8) -0.0021(8) C2 0.0380(10) 0.0641(13) 0.0440(11) 0.0038(10) 0.0070(8) 0.0007(9) C3 0.0454(12) 0.0946(19) 0.0465(12) -0.0105(12) 0.0126(10) -0.0066(12) C4 0.0507(13) 0.0758(17) 0.0785(17) -0.0371(14) 0.0194(12) -0.0064(12) C5 0.0438(11) 0.0534(12) 0.0710(15) -0.0161(11) 0.0156(10) -0.0094(10) C6 0.0558(12) 0.0464(12) 0.0619(13) -0.0024(10) 0.0196(10) 0.0059(10) C7 0.0700(16) 0.0582(15) 0.0911(19) -0.0256(14) 0.0129(14) -0.0047(12) C8 0.092(2) 0.0710(17) 0.0880(19) -0.0099(15) 0.0433(16) 0.0153(15) C9 0.090(2) 0.0562(15) 0.091(2) 0.0143(14) 0.0283(16) 0.0131(13) C10 0.0348(11) 0.0776(16) 0.0624(14) 0.0007(12) 0.0054(10) -0.0039(10) C11 0.0636(16) 0.132(3) 0.0571(15) 0.0077(16) -0.0068(13) -0.0112(16) C12 0.0534(15) 0.088(2) 0.099(2) -0.0174(16) 0.0048(14) -0.0229(14) C13 0.0379(13) 0.119(3) 0.109(2) 0.0005(19) 0.0150(14) 0.0031(14) C14 0.144(3) 0.0485(15) 0.088(2) -0.0018(14) 0.000(2) -0.0022(17) C15 0.091(2) 0.130(3) 0.101(3) 0.015(2) 0.048(2) -0.017(2) C16 0.097(2) 0.0729(17) 0.0547(14) -0.0020(13) 0.0097(14) -0.0058(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 Fe1 C5 2.020(2) 2 ? Fe1 C5 2.020(2) . ? Fe1 C4 2.029(2) 2 ? Fe1 C4 2.029(2) . ? Fe1 C3 2.048(2) . ? Fe1 C3 2.048(2) 2 ? Fe1 C2 2.053(2) 2 ? Fe1 C2 2.053(2) . ? Fe1 C1 2.0558(19) 2 ? Fe1 C1 2.0558(19) . ? P1 N1 1.5234(19) . ? P1 C1 1.807(2) . ? P1 C6 1.871(2) . ? P1 C10 1.880(2) . ? N1 Si1 1.6469(19) . ? Si1 C15 1.869(3) . ? Si1 C14 1.871(3) . ? Si1 C16 1.871(3) . ? C1 C5 1.432(3) . ? C1 C2 1.433(3) . ? C2 C3 1.416(3) . ? C3 C4 1.395(4) . ? C4 C5 1.412(3) . ? C6 C7 1.532(3) . ? C6 C8 1.535(3) . ? C6 C9 1.536(3) . ? C10 C11 1.530(3) . ? C10 C13 1.534(4) . ? C10 C12 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 C5 Fe1 C5 118.46(13) 2 . ? C5 Fe1 C4 40.82(9) 2 2 ? C5 Fe1 C4 102.89(10) . 2 ? C5 Fe1 C4 102.89(10) 2 . ? C5 Fe1 C4 40.82(9) . . ? C4 Fe1 C4 117.13(17) 2 . ? C5 Fe1 C3 119.99(10) 2 . ? C5 Fe1 C3 68.12(10) . . ? C4 Fe1 C3 153.56(12) 2 . ? C4 Fe1 C3 40.02(11) . . ? C5 Fe1 C3 68.12(10) 2 2 ? C5 Fe1 C3 119.99(10) . 2 ? C4 Fe1 C3 40.02(11) 2 2 ? C4 Fe1 C3 153.56(12) . 2 ? C3 Fe1 C3 165.73(16) . 2 ? C5 Fe1 C2 68.42(9) 2 2 ? C5 Fe1 C2 158.01(9) . 2 ? C4 Fe1 C2 67.90(10) 2 2 ? C4 Fe1 C2 161.16(9) . 2 ? C3 Fe1 C2 128.73(10) . 2 ? C3 Fe1 C2 40.40(9) 2 2 ? C5 Fe1 C2 158.02(9) 2 . ? C5 Fe1 C2 68.42(9) . . ? C4 Fe1 C2 161.16(9) 2 . ? C4 Fe1 C2 67.91(10) . . ? C3 Fe1 C2 40.40(9) . . ? C3 Fe1 C2 128.73(10) 2 . ? C2 Fe1 C2 113.71(13) 2 . ? C5 Fe1 C1 41.12(8) 2 2 ? C5 Fe1 C1 156.47(9) . 2 ? C4 Fe1 C1 68.83(9) 2 2 ? C4 Fe1 C1 121.86(9) . 2 ? C3 Fe1 C1 109.04(9) . 2 ? C3 Fe1 C1 68.53(8) 2 2 ? C2 Fe1 C1 40.82(8) 2 2 ? C2 Fe1 C1 125.60(8) . 2 ? C5 Fe1 C1 156.47(9) 2 . ? C5 Fe1 C1 41.12(8) . . ? C4 Fe1 C1 121.86(9) 2 . ? C4 Fe1 C1 68.83(9) . . ? C3 Fe1 C1 68.53(8) . . ? C3 Fe1 C1 109.04(8) 2 . ? C2 Fe1 C1 125.60(8) 2 . ? C2 Fe1 C1 40.81(8) . . ? C1 Fe1 C1 161.61(11) 2 . ? N1 P1 C1 111.47(10) . . ? N1 P1 C6 110.77(11) . . ? C1 P1 C6 109.17(10) . . ? N1 P1 C10 112.61(11) . . ? C1 P1 C10 101.27(10) . . ? C6 P1 C10 111.17(11) . . ? P1 N1 Si1 171.59(15) . . ? N1 Si1 C15 111.96(14) . . ? N1 Si1 C14 111.65(13) . . ? C15 Si1 C14 107.77(17) . . ? N1 Si1 C16 110.17(12) . . ? C15 Si1 C16 107.98(15) . . ? C14 Si1 C16 107.10(14) . . ? C5 C1 C2 106.16(18) . . ? C5 C1 P1 120.44(16) . . ? C2 C1 P1 132.77(16) . . ? C5 C1 Fe1 68.09(11) . . ? C2 C1 Fe1 69.51(11) . . ? P1 C1 Fe1 133.53(11) . . ? C3 C2 C1 108.4(2) . . ? C3 C2 Fe1 69.61(13) . . ? C1 C2 Fe1 69.68(11) . . ? C4 C3 C2 108.4(2) . . ? C4 C3 Fe1 69.24(15) . . ? C2 C3 Fe1 69.99(12) . . ? C3 C4 C5 108.5(2) . . ? C3 C4 Fe1 70.74(13) . . ? C5 C4 Fe1 69.24(13) . . ? C4 C5 C1 108.6(2) . . ? C4 C5 Fe1 69.94(13) . . ? C1 C5 Fe1 70.79(11) . . ? C7 C6 C8 106.8(2) . . ? C7 C6 C9 109.2(2) . . ? C8 C6 C9 109.2(2) . . ? C7 C6 P1 108.00(15) . . ? C8 C6 P1 108.18(16) . . ? C9 C6 P1 115.15(17) . . ? C11 C10 C13 110.6(2) . . ? C11 C10 C12 108.2(2) . . ? C13 C10 C12 107.5(2) . . ? C11 C10 P1 113.38(16) . . ? C13 C10 P1 110.42(19) . . ? C12 C10 P1 106.49(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.297 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.044 #===end data_CpFe(C5H3(PBu2N)2TiCl2 _database_code_depnum_ccdc_archive 'CCDC 747512' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H48 Cl6 Fe N2 P2 Ti' _chemical_formula_weight 791.07 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 19.361(4) _cell_length_b 10.900(2) _cell_length_c 17.105(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.55(3) _cell_angle_gamma 90.00 _cell_volume 3569.8(12) _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 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 0.829 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 12144 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4060 _reflns_number_gt 3431 _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 Rfactors 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^)+(0.0380P)^2^+5.6284P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 4060 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Fe1 Fe 0.0000 0.26953(4) 0.2500 0.01558(10) Uani 1 2 d S . . Ti1 Ti 0.0000 -0.15677(4) 0.2500 0.01294(11) Uani 1 2 d S . . Cl1 Cl 0.04659(3) -0.27902(5) 0.16113(3) 0.03027(14) Uani 1 1 d . . . Cl11 Cl 0.09442(3) -0.45789(5) 0.01319(3) 0.03179(14) Uani 1 1 d . . . Cl22 Cl 0.17072(4) -0.59173(6) -0.09440(4) 0.04614(18) Uani 1 1 d . . . P1 P -0.12141(2) 0.04244(4) 0.16870(3) 0.01388(11) Uani 1 1 d . . . N1 N -0.06922(8) -0.06579(15) 0.19870(10) 0.0171(3) Uani 1 1 d . . . C1 C -0.09912(10) 0.31012(19) 0.19451(13) 0.0212(4) Uani 1 1 d . . . H1A H -0.1113 0.3389 0.1399 0.025 Uiso 1 1 calc R . . C2 C -0.09515(9) 0.18409(18) 0.21945(11) 0.0164(4) Uani 1 1 d . . . C3 C -0.07413(9) 0.1850(2) 0.30362(11) 0.0190(4) Uani 1 1 d . . . H3A H -0.0668 0.1123 0.3376 0.023 Uiso 1 1 calc R . . C4 C -0.06598(10) 0.3085(2) 0.32944(13) 0.0244(4) Uani 1 1 d . . . H4A H -0.0521 0.3358 0.3841 0.029 Uiso 1 1 calc R . . C5 C -0.08101(11) 0.3858(2) 0.26205(14) 0.0262(5) Uani 1 1 d . . . H5A H -0.0790 0.4756 0.2622 0.031 Uiso 1 1 calc R . . C6 C -0.20941(10) 0.01145(19) 0.19761(12) 0.0184(4) Uani 1 1 d . . . C7 C -0.25579(11) 0.1261(2) 0.19109(14) 0.0270(5) Uani 1 1 d . . . H7A H -0.3002 0.1060 0.2064 0.041 Uiso 1 1 calc R . . H7B H -0.2626 0.1550 0.1375 0.041 Uiso 1 1 calc R . . H7C H -0.2336 0.1889 0.2253 0.041 Uiso 1 1 calc R . . C8 C -0.19764(11) -0.0309(2) 0.28429(13) 0.0261(5) Uani 1 1 d . . . H8A H -0.2419 -0.0476 0.3010 0.039 Uiso 1 1 calc R . . H8B H -0.1740 0.0325 0.3169 0.039 Uiso 1 1 calc R . . H8C H -0.1697 -0.1040 0.2891 0.039 Uiso 1 1 calc R . . C9 C -0.24565(11) -0.0938(2) 0.14737(13) 0.0252(5) Uani 1 1 d . . . H9A H -0.2906 -0.1089 0.1626 0.038 Uiso 1 1 calc R . . H9B H -0.2176 -0.1666 0.1556 0.038 Uiso 1 1 calc R . . H9C H -0.2513 -0.0714 0.0925 0.038 Uiso 1 1 calc R . . C10 C -0.12473(10) 0.06074(19) 0.05965(11) 0.0193(4) Uani 1 1 d . . . C11 C -0.18529(11) 0.1409(2) 0.02075(12) 0.0260(5) Uani 1 1 d . . . H11A H -0.1838 0.1464 -0.0350 0.039 Uiso 1 1 calc R . . H11B H -0.1811 0.2216 0.0435 0.039 Uiso 1 1 calc R . . H11C H -0.2288 0.1051 0.0293 0.039 Uiso 1 1 calc R . . C12 C -0.12884(11) -0.0673(2) 0.02135(12) 0.0247(5) Uani 1 1 d . . . H12A H -0.1306 -0.0591 -0.0348 0.037 Uiso 1 1 calc R . . H12B H -0.1701 -0.1085 0.0324 0.037 Uiso 1 1 calc R . . H12C H -0.0884 -0.1141 0.0426 0.037 Uiso 1 1 calc R . . C13 C -0.05539(11) 0.1184(2) 0.04472(12) 0.0230(4) Uani 1 1 d . . . H13A H -0.0559 0.1288 -0.0111 0.035 Uiso 1 1 calc R . . H13B H -0.0174 0.0657 0.0656 0.035 Uiso 1 1 calc R . . H13C H -0.0496 0.1969 0.0704 0.035 Uiso 1 1 calc R . . C51 C 0.10122(19) -0.5924(3) -0.0409(2) 0.0671(11) Uani 1 1 d . . . H51A H 0.1065 -0.6615 -0.0048 0.081 Uiso 1 1 calc R . . H51B H 0.0582 -0.6041 -0.0772 0.081 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 Fe1 0.01395(19) 0.0136(2) 0.0201(2) 0.000 0.00570(14) 0.000 Ti1 0.0128(2) 0.0123(2) 0.0134(2) 0.000 0.00065(16) 0.000 Cl1 0.0297(3) 0.0319(3) 0.0290(3) -0.0127(2) 0.0036(2) 0.0078(2) Cl11 0.0367(3) 0.0280(3) 0.0315(3) -0.0029(2) 0.0079(2) -0.0002(2) Cl22 0.0565(4) 0.0392(4) 0.0479(4) 0.0009(3) 0.0245(3) 0.0117(3) P1 0.0120(2) 0.0152(2) 0.0145(2) 0.00117(18) 0.00225(16) 0.00176(18) N1 0.0153(8) 0.0174(8) 0.0186(8) 0.0012(6) 0.0024(6) 0.0011(6) C1 0.0167(9) 0.0185(10) 0.0290(11) 0.0010(8) 0.0050(8) 0.0039(8) C2 0.0136(8) 0.0169(9) 0.0196(9) -0.0004(8) 0.0052(7) 0.0002(7) C3 0.0140(9) 0.0249(10) 0.0195(10) -0.0017(8) 0.0071(7) -0.0027(8) C4 0.0185(9) 0.0299(11) 0.0266(11) -0.0098(9) 0.0096(8) 0.0000(9) C5 0.0195(10) 0.0184(10) 0.0414(13) -0.0070(9) 0.0066(9) 0.0043(8) C6 0.0120(8) 0.0212(10) 0.0227(10) -0.0015(8) 0.0051(7) -0.0013(8) C7 0.0171(10) 0.0275(11) 0.0375(12) -0.0009(10) 0.0072(8) 0.0048(9) C8 0.0196(10) 0.0358(13) 0.0248(11) 0.0025(9) 0.0095(8) -0.0049(9) C9 0.0178(10) 0.0259(11) 0.0324(12) -0.0044(9) 0.0053(8) -0.0051(8) C10 0.0190(9) 0.0234(10) 0.0154(9) 0.0011(8) 0.0020(7) 0.0038(8) C11 0.0252(10) 0.0296(12) 0.0216(10) 0.0059(9) -0.0020(8) 0.0070(9) C12 0.0274(11) 0.0281(11) 0.0184(10) -0.0037(8) 0.0028(8) 0.0022(9) C13 0.0237(10) 0.0289(11) 0.0179(10) 0.0025(8) 0.0079(8) 0.0004(9) C51 0.075(2) 0.057(2) 0.081(2) -0.0451(19) 0.0519(19) -0.0414(18) _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 Fe1 C3 2.0353(19) . ? Fe1 C3 2.0354(19) 2 ? Fe1 C4 2.043(2) 2 ? Fe1 C4 2.043(2) . ? Fe1 C5 2.050(2) 2 ? Fe1 C5 2.050(2) . ? Fe1 C1 2.059(2) 2 ? Fe1 C1 2.059(2) . ? Fe1 C2 2.0610(19) 2 ? Fe1 C2 2.0611(19) . ? Ti1 N1 1.7888(16) . ? Ti1 N1 1.7889(16) 2 ? Ti1 Cl1 2.3038(7) . ? Ti1 Cl1 2.3038(7) 2 ? Cl11 C51 1.750(3) . ? Cl22 C51 1.736(3) . ? P1 N1 1.5881(17) . ? P1 C2 1.807(2) . ? P1 C10 1.867(2) . ? P1 C6 1.8740(19) . ? C1 C5 1.421(3) . ? C1 C2 1.437(3) . ? C2 C3 1.437(3) . ? C3 C4 1.419(3) . ? C4 C5 1.422(3) . ? C6 C7 1.533(3) . ? C6 C8 1.537(3) . ? C6 C9 1.538(3) . ? C10 C11 1.533(3) . ? C10 C13 1.538(3) . ? C10 C12 1.538(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 C3 Fe1 C3 126.14(12) . 2 ? C3 Fe1 C4 161.14(9) . 2 ? C3 Fe1 C4 40.71(8) 2 2 ? C3 Fe1 C4 40.71(8) . . ? C3 Fe1 C4 161.15(9) 2 . ? C4 Fe1 C4 156.01(13) 2 . ? C3 Fe1 C5 157.88(9) . 2 ? C3 Fe1 C5 68.50(9) 2 2 ? C4 Fe1 C5 40.67(9) 2 2 ? C4 Fe1 C5 120.11(9) . 2 ? C3 Fe1 C5 68.49(9) . . ? C3 Fe1 C5 157.88(9) 2 . ? C4 Fe1 C5 120.11(9) 2 . ? C4 Fe1 C5 40.67(9) . . ? C5 Fe1 C5 103.66(12) 2 . ? C3 Fe1 C1 124.13(8) . 2 ? C3 Fe1 C1 68.51(8) 2 2 ? C4 Fe1 C1 68.28(9) 2 2 ? C4 Fe1 C1 106.31(8) . 2 ? C5 Fe1 C1 40.45(8) 2 2 ? C5 Fe1 C1 119.70(9) . 2 ? C3 Fe1 C1 68.51(8) . . ? C3 Fe1 C1 124.13(8) 2 . ? C4 Fe1 C1 106.31(8) 2 . ? C4 Fe1 C1 68.28(9) . . ? C5 Fe1 C1 119.70(9) 2 . ? C5 Fe1 C1 40.45(8) . . ? C1 Fe1 C1 155.18(12) 2 . ? C3 Fe1 C2 110.16(8) . 2 ? C3 Fe1 C2 41.06(8) 2 2 ? C4 Fe1 C2 68.84(8) 2 2 ? C4 Fe1 C2 123.29(8) . 2 ? C5 Fe1 C2 68.69(8) 2 2 ? C5 Fe1 C2 157.22(8) . 2 ? C1 Fe1 C2 40.83(8) 2 2 ? C1 Fe1 C2 161.96(8) . 2 ? C3 Fe1 C2 41.06(8) . . ? C3 Fe1 C2 110.16(8) 2 . ? C4 Fe1 C2 123.29(8) 2 . ? C4 Fe1 C2 68.84(8) . . ? C5 Fe1 C2 157.21(8) 2 . ? C5 Fe1 C2 68.69(8) . . ? C1 Fe1 C2 161.96(8) 2 . ? C1 Fe1 C2 40.83(8) . . ? C2 Fe1 C2 126.27(11) 2 . ? N1 Ti1 N1 112.66(11) . 2 ? N1 Ti1 Cl1 109.58(6) . . ? N1 Ti1 Cl1 107.82(6) 2 . ? N1 Ti1 Cl1 107.83(6) . 2 ? N1 Ti1 Cl1 109.59(6) 2 2 ? Cl1 Ti1 Cl1 109.33(4) . 2 ? N1 P1 C2 111.07(9) . . ? N1 P1 C10 109.14(9) . . ? C2 P1 C10 110.74(9) . . ? N1 P1 C6 109.91(9) . . ? C2 P1 C6 103.25(9) . . ? C10 P1 C6 112.65(9) . . ? P1 N1 Ti1 164.72(11) . . ? C5 C1 C2 108.52(19) . . ? C5 C1 Fe1 69.46(12) . . ? C2 C1 Fe1 69.67(11) . . ? C3 C2 C1 106.61(17) . . ? C3 C2 P1 120.31(15) . . ? C1 C2 P1 132.48(15) . . ? C3 C2 Fe1 68.51(11) . . ? C1 C2 Fe1 69.50(11) . . ? P1 C2 Fe1 133.24(10) . . ? C4 C3 C2 108.66(18) . . ? C4 C3 Fe1 69.94(11) . . ? C2 C3 Fe1 70.43(11) . . ? C3 C4 C5 108.06(18) . . ? C3 C4 Fe1 69.35(11) . . ? C5 C4 Fe1 69.94(12) . . ? C1 C5 C4 108.14(19) . . ? C1 C5 Fe1 70.09(12) . . ? C4 C5 Fe1 69.40(12) . . ? C7 C6 C8 108.42(17) . . ? C7 C6 C9 110.69(17) . . ? C8 C6 C9 107.76(17) . . ? C7 C6 P1 112.31(14) . . ? C8 C6 P1 107.37(13) . . ? C9 C6 P1 110.13(14) . . ? C11 C10 C13 108.96(17) . . ? C11 C10 C12 110.16(17) . . ? C13 C10 C12 106.94(17) . . ? C11 C10 P1 113.90(14) . . ? C13 C10 P1 107.95(13) . . ? C12 C10 P1 108.69(14) . . ? Cl22 C51 Cl11 113.60(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.746 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.073 #===end data_Fe(C5H4PtBu2NTiCl3)2 _database_code_depnum_ccdc_archive 'CCDC 747513' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C26 H44 Cl6 Fe N2 P2 Ti2' _chemical_formula_weight 810.92 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 26.615(5) _cell_length_b 9.6625(19) _cell_length_c 14.696(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.29(3) _cell_angle_gamma 90.00 _cell_volume 3645.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 11621 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4156 _reflns_number_gt 2824 _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 Rfactors 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^)+(0.0424P)^2^+4.9784P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4156 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Fe1 Fe 0.5000 0.77333(6) 0.2500 0.02003(17) Uani 1 2 d S . . Ti1 Ti 0.38386(2) 0.65210(6) 0.45028(4) 0.02495(17) Uani 1 1 d . . . P1 P 0.37363(3) 0.85903(8) 0.26479(6) 0.02004(19) Uani 1 1 d . . . Cl2 Cl 0.44692(3) 0.72147(9) 0.57635(6) 0.0343(2) Uani 1 1 d . . . Cl1 Cl 0.30657(4) 0.65005(13) 0.48308(8) 0.0605(3) Uani 1 1 d . . . Cl3 Cl 0.40213(5) 0.44382(9) 0.40134(7) 0.0584(3) Uani 1 1 d . . . N1 N 0.38132(10) 0.7652(3) 0.35923(18) 0.0251(6) Uani 1 1 d . . . C10 C 0.37944(12) 1.0439(3) 0.3013(2) 0.0238(7) Uani 1 1 d . . . C2 C 0.44742(12) 0.8874(3) 0.1490(2) 0.0225(7) Uani 1 1 d . . . H2A H 0.4470 0.9884 0.1429 0.027 Uiso 1 1 calc R . . C4 C 0.46599(13) 0.6586(3) 0.1328(2) 0.0278(8) Uani 1 1 d . . . H4A H 0.4803 0.5739 0.1129 0.033 Uiso 1 1 calc R . . C6 C 0.30996(12) 0.8133(3) 0.1815(2) 0.0278(8) Uani 1 1 d . . . C1 C 0.42141(12) 0.8090(3) 0.2054(2) 0.0212(7) Uani 1 1 d . . . C13 C 0.35765(14) 1.1435(3) 0.2188(2) 0.0320(8) Uani 1 1 d . . . H13A H 0.3616 1.2371 0.2413 0.048 Uiso 1 1 calc R . . H13B H 0.3214 1.1241 0.1918 0.048 Uiso 1 1 calc R . . H13C H 0.3763 1.1313 0.1717 0.048 Uiso 1 1 calc R . . C3 C 0.47471(12) 0.7940(3) 0.1048(2) 0.0256(7) Uani 1 1 d . . . H3A H 0.4964 0.8195 0.0629 0.031 Uiso 1 1 calc R . . C5 C 0.43364(12) 0.6652(3) 0.1946(2) 0.0267(7) Uani 1 1 d . . . H5A H 0.4210 0.5861 0.2240 0.032 Uiso 1 1 calc R . . C12 C 0.35111(14) 1.0648(3) 0.3785(2) 0.0322(8) Uani 1 1 d . . . H12A H 0.3537 1.1600 0.3978 0.048 Uiso 1 1 calc R . . H12B H 0.3668 1.0072 0.4317 0.048 Uiso 1 1 calc R . . H12C H 0.3151 1.0402 0.3545 0.048 Uiso 1 1 calc R . . C7 C 0.30656(14) 0.8714(4) 0.0832(2) 0.0374(9) Uani 1 1 d . . . H7A H 0.2736 0.8468 0.0411 0.056 Uiso 1 1 calc R . . H7B H 0.3342 0.8335 0.0601 0.056 Uiso 1 1 calc R . . H7C H 0.3097 0.9703 0.0866 0.056 Uiso 1 1 calc R . . C11 C 0.43746(13) 1.0758(3) 0.3448(3) 0.0318(8) Uani 1 1 d . . . H11A H 0.4414 1.1710 0.3640 0.048 Uiso 1 1 calc R . . H11B H 0.4566 1.0587 0.2990 0.048 Uiso 1 1 calc R . . H11C H 0.4506 1.0174 0.3987 0.048 Uiso 1 1 calc R . . C8 C 0.30664(14) 0.6541(3) 0.1756(3) 0.0361(9) Uani 1 1 d . . . H8A H 0.2741 0.6274 0.1330 0.054 Uiso 1 1 calc R . . H8B H 0.3088 0.6169 0.2371 0.054 Uiso 1 1 calc R . . H8C H 0.3349 0.6190 0.1531 0.054 Uiso 1 1 calc R . . C9 C 0.26470(13) 0.8670(4) 0.2186(3) 0.0396(9) Uani 1 1 d . . . H9A H 0.2322 0.8427 0.1750 0.059 Uiso 1 1 calc R . . H9B H 0.2671 0.9658 0.2250 0.059 Uiso 1 1 calc R . . H9C H 0.2666 0.8261 0.2789 0.059 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 Fe1 0.0177(3) 0.0187(3) 0.0236(4) 0.000 0.0052(3) 0.000 Ti1 0.0269(3) 0.0217(3) 0.0253(3) 0.0004(2) 0.0052(3) -0.0037(2) P1 0.0161(4) 0.0205(4) 0.0231(5) -0.0005(3) 0.0043(3) -0.0013(3) Cl2 0.0333(5) 0.0339(5) 0.0322(5) -0.0044(4) 0.0022(4) -0.0036(4) Cl1 0.0345(6) 0.0967(9) 0.0545(7) 0.0094(6) 0.0192(5) -0.0144(6) Cl3 0.0974(9) 0.0225(5) 0.0446(6) -0.0051(4) 0.0000(6) 0.0078(5) N1 0.0222(15) 0.0245(14) 0.0288(15) 0.0005(11) 0.0069(12) 0.0002(11) C10 0.0227(17) 0.0195(16) 0.0284(18) -0.0010(13) 0.0053(14) 0.0016(13) C2 0.0186(16) 0.0259(16) 0.0234(17) 0.0037(13) 0.0062(14) 0.0012(13) C4 0.0250(18) 0.0285(18) 0.0280(19) -0.0133(14) 0.0036(15) -0.0034(14) C6 0.0164(16) 0.0375(19) 0.0283(19) -0.0008(14) 0.0035(14) -0.0047(14) C1 0.0173(16) 0.0225(16) 0.0221(17) -0.0031(12) 0.0025(13) -0.0002(12) C13 0.034(2) 0.0250(18) 0.037(2) 0.0031(14) 0.0098(17) 0.0028(15) C3 0.0222(17) 0.0325(18) 0.0228(17) -0.0020(14) 0.0072(14) -0.0011(14) C5 0.0226(18) 0.0240(17) 0.033(2) -0.0051(13) 0.0066(15) -0.0061(13) C12 0.030(2) 0.0298(19) 0.038(2) -0.0054(15) 0.0129(17) 0.0033(15) C7 0.028(2) 0.052(2) 0.027(2) -0.0009(16) -0.0018(16) -0.0093(17) C11 0.0260(19) 0.0264(18) 0.041(2) -0.0116(15) 0.0057(16) -0.0039(14) C8 0.0257(19) 0.040(2) 0.039(2) -0.0045(16) 0.0013(17) -0.0122(16) C9 0.0192(19) 0.053(2) 0.046(2) -0.0020(18) 0.0067(17) -0.0030(16) _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 Fe1 C5 2.029(3) 2_655 ? Fe1 C5 2.029(3) . ? Fe1 C4 2.048(3) 2_655 ? Fe1 C4 2.048(3) . ? Fe1 C1 2.050(3) . ? Fe1 C1 2.050(3) 2_655 ? Fe1 C2 2.069(3) . ? Fe1 C2 2.069(3) 2_655 ? Fe1 C3 2.071(3) . ? Fe1 C3 2.071(3) 2_655 ? Ti1 N1 1.715(3) . ? Ti1 Cl1 2.2332(13) . ? Ti1 Cl3 2.2335(11) . ? Ti1 Cl2 2.2492(13) . ? P1 N1 1.625(3) . ? P1 C1 1.788(3) . ? P1 C10 1.860(3) . ? P1 C6 1.864(3) . ? C10 C12 1.532(4) . ? C10 C13 1.537(4) . ? C10 C11 1.539(4) . ? C2 C3 1.419(4) . ? C2 C1 1.429(4) . ? C4 C5 1.408(5) . ? C4 C3 1.409(5) . ? C6 C7 1.530(5) . ? C6 C9 1.538(5) . ? C6 C8 1.541(5) . ? C1 C5 1.445(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 C5 Fe1 C5 118.03(18) 2_655 . ? C5 Fe1 C4 40.41(13) 2_655 2_655 ? C5 Fe1 C4 101.78(14) . 2_655 ? C5 Fe1 C4 101.78(14) 2_655 . ? C5 Fe1 C4 40.41(13) . . ? C4 Fe1 C4 114.47(19) 2_655 . ? C5 Fe1 C1 157.23(13) 2_655 . ? C5 Fe1 C1 41.51(12) . . ? C4 Fe1 C1 123.19(13) 2_655 . ? C4 Fe1 C1 68.57(13) . . ? C5 Fe1 C1 41.51(12) 2_655 2_655 ? C5 Fe1 C1 157.23(12) . 2_655 ? C4 Fe1 C1 68.57(13) 2_655 2_655 ? C4 Fe1 C1 123.19(13) . 2_655 ? C1 Fe1 C1 160.63(17) . 2_655 ? C5 Fe1 C2 156.20(13) 2_655 . ? C5 Fe1 C2 68.51(13) . . ? C4 Fe1 C2 163.17(12) 2_655 . ? C4 Fe1 C2 67.64(13) . . ? C1 Fe1 C2 40.61(12) . . ? C1 Fe1 C2 125.45(12) 2_655 . ? C5 Fe1 C2 68.51(13) 2_655 2_655 ? C5 Fe1 C2 156.20(13) . 2_655 ? C4 Fe1 C2 67.64(13) 2_655 2_655 ? C4 Fe1 C2 163.16(12) . 2_655 ? C1 Fe1 C2 125.45(12) . 2_655 ? C1 Fe1 C2 40.61(12) 2_655 2_655 ? C2 Fe1 C2 115.61(18) . 2_655 ? C5 Fe1 C3 118.39(13) 2_655 . ? C5 Fe1 C3 67.91(13) . . ? C4 Fe1 C3 150.53(13) 2_655 . ? C4 Fe1 C3 40.00(13) . . ? C1 Fe1 C3 68.12(13) . . ? C1 Fe1 C3 109.88(13) 2_655 . ? C2 Fe1 C3 40.08(12) . . ? C2 Fe1 C3 131.46(13) 2_655 . ? C5 Fe1 C3 67.91(13) 2_655 2_655 ? C5 Fe1 C3 118.39(13) . 2_655 ? C4 Fe1 C3 40.00(13) 2_655 2_655 ? C4 Fe1 C3 150.53(13) . 2_655 ? C1 Fe1 C3 109.88(13) . 2_655 ? C1 Fe1 C3 68.12(13) 2_655 2_655 ? C2 Fe1 C3 131.46(13) . 2_655 ? C2 Fe1 C3 40.08(12) 2_655 2_655 ? C3 Fe1 C3 168.91(18) . 2_655 ? N1 Ti1 Cl1 108.97(10) . . ? N1 Ti1 Cl3 106.87(9) . . ? Cl1 Ti1 Cl3 110.65(5) . . ? N1 Ti1 Cl2 108.66(9) . . ? Cl1 Ti1 Cl2 110.77(5) . . ? Cl3 Ti1 Cl2 110.81(4) . . ? N1 P1 C1 108.69(14) . . ? N1 P1 C10 107.89(14) . . ? C1 P1 C10 112.62(14) . . ? N1 P1 C6 108.47(14) . . ? C1 P1 C6 104.82(14) . . ? C10 P1 C6 114.17(15) . . ? P1 N1 Ti1 172.76(18) . . ? C12 C10 C13 110.2(3) . . ? C12 C10 C11 107.6(3) . . ? C13 C10 C11 109.4(3) . . ? C12 C10 P1 108.7(2) . . ? C13 C10 P1 112.8(2) . . ? C11 C10 P1 108.0(2) . . ? C3 C2 C1 108.3(3) . . ? C3 C2 Fe1 70.04(18) . . ? C1 C2 Fe1 68.96(17) . . ? C5 C4 C3 108.8(3) . . ? C5 C4 Fe1 69.07(18) . . ? C3 C4 Fe1 70.89(18) . . ? C7 C6 C9 110.7(3) . . ? C7 C6 C8 109.0(3) . . ? C9 C6 C8 108.6(3) . . ? C7 C6 P1 110.5(2) . . ? C9 C6 P1 110.4(2) . . ? C8 C6 P1 107.6(2) . . ? C2 C1 C5 106.7(3) . . ? C2 C1 P1 130.9(2) . . ? C5 C1 P1 121.6(2) . . ? C2 C1 Fe1 70.43(18) . . ? C5 C1 Fe1 68.47(17) . . ? P1 C1 Fe1 133.37(17) . . ? C4 C3 C2 108.3(3) . . ? C4 C3 Fe1 69.11(18) . . ? C2 C3 Fe1 69.88(18) . . ? C4 C5 C1 108.0(3) . . ? C4 C5 Fe1 70.52(18) . . ? C1 C5 Fe1 70.02(17) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.752 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.102 #===end data_Fe(5-C5H4PtBu2NTiCp*Cl2)2 _database_code_depnum_ccdc_archive 'CCDC 747514' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C48 H76 Cl10 Fe N2 P2 Ti2' _chemical_formula_weight 1249.20 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' Fe Fe 0.3463 0.8444 '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 8.6321(17) _cell_length_b 18.488(4) _cell_length_c 18.445(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.45(3) _cell_angle_gamma 90.00 _cell_volume 2874.3(10) _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 0.19 _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type none _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 17636 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5045 _reflns_number_gt 3332 _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 Rfactors 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^)+(0.0652P)^2^+0.5778P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 5045 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Fe1 Fe 0.0000 0.0000 0.5000 0.0232(2) Uani 1 2 d S . . Ti1 Ti 0.12204(8) 0.10039(4) 0.77069(4) 0.0215(2) Uani 1 1 d . . . P1 P 0.14438(11) 0.16461(6) 0.60270(6) 0.0213(3) Uani 1 1 d . . . N1 N 0.1543(3) 0.13934(17) 0.68679(17) 0.0220(8) Uani 1 1 d . . . C1 C 0.3546(4) 0.0960(2) 0.8665(2) 0.0291(10) Uani 1 1 d . . . C2 C 0.2317(5) 0.0713(2) 0.9020(2) 0.0290(10) Uani 1 1 d . . . C3 C 0.1266(4) 0.1294(2) 0.9013(2) 0.0291(10) Uani 1 1 d . . . C4 C 0.1798(5) 0.1891(2) 0.8648(2) 0.0275(10) Uani 1 1 d . . . C5 C 0.3239(4) 0.1681(2) 0.8452(2) 0.0281(10) Uani 1 1 d . . . C6 C 0.4981(5) 0.0527(3) 0.8596(3) 0.0464(13) Uani 1 1 d . . . H6A H 0.5789 0.0580 0.9040 0.070 Uiso 1 1 calc R . . H6B H 0.5374 0.0698 0.8178 0.070 Uiso 1 1 calc R . . H6C H 0.4695 0.0026 0.8525 0.070 Uiso 1 1 calc R . . C7 C 0.2239(6) -0.0014(3) 0.9369(3) 0.0452(13) Uani 1 1 d . . . H7A H 0.2748 0.0009 0.9886 0.068 Uiso 1 1 calc R . . H7B H 0.2770 -0.0365 0.9125 0.068 Uiso 1 1 calc R . . H7C H 0.1150 -0.0153 0.9321 0.068 Uiso 1 1 calc R . . C8 C -0.0153(5) 0.1295(3) 0.9367(3) 0.0469(13) Uani 1 1 d . . . H8A H 0.0176 0.1427 0.9881 0.070 Uiso 1 1 calc R . . H8B H -0.0619 0.0821 0.9329 0.070 Uiso 1 1 calc R . . H8C H -0.0921 0.1638 0.9118 0.070 Uiso 1 1 calc R . . C9 C 0.1077(6) 0.2632(3) 0.8578(3) 0.0463(13) Uani 1 1 d . . . H9A H 0.1478 0.2901 0.9025 0.070 Uiso 1 1 calc R . . H9B H -0.0056 0.2592 0.8502 0.070 Uiso 1 1 calc R . . H9C H 0.1346 0.2878 0.8164 0.070 Uiso 1 1 calc R . . C10 C 0.4324(5) 0.2160(3) 0.8129(2) 0.0439(13) Uani 1 1 d . . . H10A H 0.5068 0.2391 0.8524 0.066 Uiso 1 1 calc R . . H10B H 0.3710 0.2522 0.7821 0.066 Uiso 1 1 calc R . . H10C H 0.4888 0.1874 0.7836 0.066 Uiso 1 1 calc R . . C11 C 0.0407(4) 0.2539(2) 0.5876(2) 0.0266(10) Uani 1 1 d . . . C12 C 0.1091(5) 0.3057(2) 0.6516(2) 0.0348(11) Uani 1 1 d . . . H12A H 0.0551 0.3513 0.6433 0.052 Uiso 1 1 calc R . . H12B H 0.2202 0.3128 0.6538 0.052 Uiso 1 1 calc R . . H12C H 0.0948 0.2854 0.6976 0.052 Uiso 1 1 calc R . . C13 C -0.1346(4) 0.2393(2) 0.5901(2) 0.0343(11) Uani 1 1 d . . . H13A H -0.1931 0.2838 0.5826 0.051 Uiso 1 1 calc R . . H13B H -0.1400 0.2194 0.6376 0.051 Uiso 1 1 calc R . . H13C H -0.1795 0.2056 0.5517 0.051 Uiso 1 1 calc R . . C14 C 0.0467(5) 0.2882(3) 0.5128(2) 0.0389(12) Uani 1 1 d . . . H14A H -0.0082 0.3337 0.5081 0.058 Uiso 1 1 calc R . . H14B H -0.0033 0.2566 0.4734 0.058 Uiso 1 1 calc R . . H14C H 0.1552 0.2959 0.5100 0.058 Uiso 1 1 calc R . . C15 C 0.3446(4) 0.1650(2) 0.5802(2) 0.0261(10) Uani 1 1 d . . . C16 C 0.4367(5) 0.2339(2) 0.6095(3) 0.0358(11) Uani 1 1 d . . . H16A H 0.5393 0.2328 0.5973 0.054 Uiso 1 1 calc R . . H16B H 0.4492 0.2363 0.6625 0.054 Uiso 1 1 calc R . . H16C H 0.3792 0.2755 0.5872 0.054 Uiso 1 1 calc R . . C17 C 0.3363(5) 0.1592(3) 0.4960(2) 0.0363(11) Uani 1 1 d . . . H17A H 0.4418 0.1596 0.4871 0.054 Uiso 1 1 calc R . . H17B H 0.2777 0.1995 0.4711 0.054 Uiso 1 1 calc R . . H17C H 0.2843 0.1150 0.4775 0.054 Uiso 1 1 calc R . . C18 C 0.4330(4) 0.0997(2) 0.6199(2) 0.0289(10) Uani 1 1 d . . . H18A H 0.5375 0.0976 0.6099 0.043 Uiso 1 1 calc R . . H18B H 0.3762 0.0562 0.6022 0.043 Uiso 1 1 calc R . . H18C H 0.4407 0.1042 0.6724 0.043 Uiso 1 1 calc R . . C19 C 0.0118(4) 0.1045(2) 0.5401(2) 0.0219(9) Uani 1 1 d . . . C20 C -0.0335(5) 0.1041(2) 0.4604(2) 0.0271(10) Uani 1 1 d . . . H20A H 0.0248 0.1273 0.4267 0.032 Uiso 1 1 calc R . . C21 C -0.1761(4) 0.0643(2) 0.4388(2) 0.0298(10) Uani 1 1 d . . . H21A H -0.2334 0.0552 0.3877 0.036 Uiso 1 1 calc R . . C22 C -0.2209(4) 0.0396(2) 0.5037(2) 0.0286(10) Uani 1 1 d . . . H22A H -0.3148 0.0104 0.5053 0.034 Uiso 1 1 calc R . . C23 C -0.1077(4) 0.0646(2) 0.5664(2) 0.0247(10) Uani 1 1 d . . . H23A H -0.1099 0.0554 0.6185 0.030 Uiso 1 1 calc R . . C24 C -0.2301(5) -0.0798(3) 0.7524(3) 0.0378(12) Uani 1 1 d . . . H24A H -0.1622 -0.0431 0.7367 0.045 Uiso 1 1 calc R . . Cl1 Cl -0.15066(11) 0.11001(6) 0.75669(6) 0.0305(3) Uani 1 1 d . . . Cl2 Cl 0.14871(12) -0.02233(6) 0.74977(6) 0.0311(3) Uani 1 1 d . . . Cl3 Cl -0.20219(14) -0.07669(7) 0.84979(7) 0.0468(3) Uani 1 1 d . . . Cl4 Cl -0.17654(16) -0.16443(8) 0.72388(9) 0.0649(4) Uani 1 1 d . . . Cl5 Cl -0.42804(14) -0.06104(7) 0.70996(8) 0.0547(4) Uani 1 1 d . . . 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 Fe1 0.0194(4) 0.0270(5) 0.0216(5) -0.0052(4) 0.0008(3) 0.0008(4) Ti1 0.0192(4) 0.0256(4) 0.0198(4) 0.0000(3) 0.0040(3) -0.0014(3) P1 0.0198(5) 0.0246(6) 0.0191(6) 0.0008(5) 0.0033(4) -0.0004(4) N1 0.0201(16) 0.027(2) 0.0177(19) -0.0028(15) 0.0023(13) -0.0025(14) C1 0.023(2) 0.043(3) 0.019(2) -0.006(2) -0.0022(17) 0.003(2) C2 0.030(2) 0.035(3) 0.019(2) 0.001(2) -0.0016(18) -0.004(2) C3 0.026(2) 0.042(3) 0.019(2) 0.000(2) 0.0042(18) -0.001(2) C4 0.039(2) 0.023(2) 0.019(2) -0.0058(19) 0.0024(18) -0.0016(19) C5 0.027(2) 0.038(3) 0.018(2) -0.004(2) 0.0006(17) -0.010(2) C6 0.034(3) 0.064(4) 0.040(3) -0.004(3) 0.004(2) 0.010(2) C7 0.062(3) 0.043(3) 0.029(3) 0.006(2) 0.006(2) -0.001(2) C8 0.039(3) 0.072(4) 0.034(3) -0.007(3) 0.015(2) -0.004(3) C9 0.060(3) 0.040(3) 0.038(3) -0.008(2) 0.008(2) 0.002(2) C10 0.052(3) 0.054(3) 0.025(3) -0.003(2) 0.006(2) -0.024(2) C11 0.028(2) 0.030(2) 0.019(2) 0.001(2) 0.0002(17) -0.0002(19) C12 0.043(3) 0.024(3) 0.035(3) -0.002(2) 0.001(2) 0.001(2) C13 0.029(2) 0.033(3) 0.040(3) 0.000(2) 0.005(2) 0.006(2) C14 0.045(3) 0.034(3) 0.035(3) 0.007(2) 0.002(2) 0.003(2) C15 0.022(2) 0.035(3) 0.023(2) 0.000(2) 0.0071(17) -0.0042(19) C16 0.032(2) 0.039(3) 0.036(3) 0.001(2) 0.008(2) -0.010(2) C17 0.030(2) 0.051(3) 0.031(3) 0.001(2) 0.0133(19) -0.002(2) C18 0.024(2) 0.037(3) 0.025(2) 0.001(2) 0.0044(17) 0.0003(19) C19 0.023(2) 0.025(2) 0.019(2) -0.0020(18) 0.0056(16) 0.0020(18) C20 0.029(2) 0.031(3) 0.021(2) -0.001(2) 0.0039(17) 0.0064(19) C21 0.021(2) 0.038(3) 0.025(3) -0.007(2) -0.0064(18) 0.006(2) C22 0.0151(19) 0.035(3) 0.035(3) -0.011(2) 0.0042(18) 0.0032(18) C23 0.019(2) 0.031(3) 0.024(2) -0.010(2) 0.0047(17) 0.0025(18) C24 0.028(2) 0.040(3) 0.046(3) 0.006(2) 0.006(2) -0.001(2) Cl1 0.0213(5) 0.0396(7) 0.0310(6) -0.0001(5) 0.0069(4) -0.0013(5) Cl2 0.0334(6) 0.0284(6) 0.0317(6) -0.0024(5) 0.0078(5) -0.0011(5) Cl3 0.0438(7) 0.0495(8) 0.0461(8) 0.0046(6) 0.0076(6) -0.0020(6) Cl4 0.0540(8) 0.0532(9) 0.0802(11) -0.0215(8) -0.0016(7) 0.0215(7) Cl5 0.0406(7) 0.0418(8) 0.0704(10) -0.0050(7) -0.0127(6) 0.0112(6) _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 Fe1 C20 2.057(4) . ? Fe1 C20 2.057(4) 3_556 ? Fe1 C22 2.058(4) . ? Fe1 C22 2.058(4) 3_556 ? Fe1 C21 2.063(4) 3_556 ? Fe1 C21 2.063(4) . ? Fe1 C19 2.064(4) 3_556 ? Fe1 C19 2.064(4) . ? Fe1 C23 2.069(4) 3_556 ? Fe1 C23 2.069(4) . ? Ti1 N1 1.782(3) . ? Ti1 Cl1 2.3189(12) . ? Ti1 Cl2 2.3210(14) . ? Ti1 C5 2.336(4) . ? Ti1 C4 2.362(4) . ? Ti1 C1 2.373(4) . ? Ti1 C3 2.460(4) . ? Ti1 C2 2.463(4) . ? P1 N1 1.604(3) . ? P1 C19 1.819(4) . ? P1 C15 1.862(4) . ? P1 C11 1.869(4) . ? C1 C5 1.398(6) . ? C1 C2 1.437(6) . ? C1 C6 1.503(6) . ? C2 C3 1.405(6) . ? C2 C7 1.499(6) . ? C3 C4 1.418(6) . ? C3 C8 1.508(6) . ? C4 C5 1.422(6) . ? C4 C9 1.499(6) . ? C5 C10 1.504(6) . ? C11 C14 1.529(6) . ? C11 C12 1.536(6) . ? C11 C13 1.547(5) . ? C15 C18 1.528(6) . ? C15 C16 1.537(6) . ? C15 C17 1.542(6) . ? C19 C23 1.436(5) . ? C19 C20 1.436(6) . ? C20 C21 1.416(6) . ? C21 C22 1.410(6) . ? C22 C23 1.420(5) . ? C24 Cl4 1.744(5) . ? C24 Cl5 1.754(4) . ? C24 Cl3 1.762(5) . ? 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 C20 Fe1 C20 179.998(1) . 3_556 ? C20 Fe1 C22 67.55(17) . . ? C20 Fe1 C22 112.45(17) 3_556 . ? C20 Fe1 C22 112.45(17) . 3_556 ? C20 Fe1 C22 67.55(17) 3_556 3_556 ? C22 Fe1 C22 179.999(1) . 3_556 ? C20 Fe1 C21 139.80(16) . 3_556 ? C20 Fe1 C21 40.20(16) 3_556 3_556 ? C22 Fe1 C21 139.97(17) . 3_556 ? C22 Fe1 C21 40.03(17) 3_556 3_556 ? C20 Fe1 C21 40.20(16) . . ? C20 Fe1 C21 139.80(16) 3_556 . ? C22 Fe1 C21 40.03(17) . . ? C22 Fe1 C21 139.97(17) 3_556 . ? C21 Fe1 C21 179.999(1) 3_556 . ? C20 Fe1 C19 139.20(15) . 3_556 ? C20 Fe1 C19 40.80(15) 3_556 3_556 ? C22 Fe1 C19 111.77(15) . 3_556 ? C22 Fe1 C19 68.23(15) 3_556 3_556 ? C21 Fe1 C19 68.30(16) 3_556 3_556 ? C21 Fe1 C19 111.70(16) . 3_556 ? C20 Fe1 C19 40.80(15) . . ? C20 Fe1 C19 139.20(15) 3_556 . ? C22 Fe1 C19 68.23(15) . . ? C22 Fe1 C19 111.77(15) 3_556 . ? C21 Fe1 C19 111.70(16) 3_556 . ? C21 Fe1 C19 68.30(16) . . ? C19 Fe1 C19 180.0(2) 3_556 . ? C20 Fe1 C23 112.12(16) . 3_556 ? C20 Fe1 C23 67.88(16) 3_556 3_556 ? C22 Fe1 C23 139.74(15) . 3_556 ? C22 Fe1 C23 40.26(15) 3_556 3_556 ? C21 Fe1 C23 67.63(16) 3_556 3_556 ? C21 Fe1 C23 112.37(16) . 3_556 ? C19 Fe1 C23 40.68(15) 3_556 3_556 ? C19 Fe1 C23 139.32(15) . 3_556 ? C20 Fe1 C23 67.88(16) . . ? C20 Fe1 C23 112.12(16) 3_556 . ? C22 Fe1 C23 40.26(15) . . ? C22 Fe1 C23 139.74(15) 3_556 . ? C21 Fe1 C23 112.37(16) 3_556 . ? C21 Fe1 C23 67.63(16) . . ? C19 Fe1 C23 139.32(15) 3_556 . ? C19 Fe1 C23 40.68(15) . . ? C23 Fe1 C23 180.000(1) 3_556 . ? N1 Ti1 Cl1 102.54(10) . . ? N1 Ti1 Cl2 102.18(11) . . ? Cl1 Ti1 Cl2 101.02(5) . . ? N1 Ti1 C5 93.34(14) . . ? Cl1 Ti1 C5 129.40(11) . . ? Cl2 Ti1 C5 122.22(12) . . ? N1 Ti1 C4 108.06(15) . . ? Cl1 Ti1 C4 94.42(11) . . ? Cl2 Ti1 C4 141.99(11) . . ? C5 Ti1 C4 35.22(14) . . ? N1 Ti1 C1 113.27(15) . . ? Cl1 Ti1 C1 139.56(11) . . ? Cl2 Ti1 C1 89.54(11) . . ? C5 Ti1 C1 34.53(15) . . ? C4 Ti1 C1 57.69(14) . . ? N1 Ti1 C3 142.13(15) . . ? Cl1 Ti1 C3 83.90(10) . . ? Cl2 Ti1 C3 113.27(11) . . ? C5 Ti1 C3 56.93(14) . . ? C4 Ti1 C3 34.14(14) . . ? C1 Ti1 C3 56.35(13) . . ? N1 Ti1 C2 147.51(14) . . ? Cl1 Ti1 C2 106.97(11) . . ? Cl2 Ti1 C2 85.37(11) . . ? C5 Ti1 C2 57.20(14) . . ? C4 Ti1 C2 56.84(14) . . ? C1 Ti1 C2 34.50(13) . . ? C3 Ti1 C2 33.16(14) . . ? N1 P1 C19 109.36(18) . . ? N1 P1 C15 110.98(17) . . ? C19 P1 C15 110.35(18) . . ? N1 P1 C11 108.95(17) . . ? C19 P1 C11 103.24(18) . . ? C15 P1 C11 113.65(19) . . ? P1 N1 Ti1 166.2(2) . . ? C5 C1 C2 108.5(4) . . ? C5 C1 C6 126.4(4) . . ? C2 C1 C6 124.9(4) . . ? C5 C1 Ti1 71.3(2) . . ? C2 C1 Ti1 76.2(2) . . ? C6 C1 Ti1 122.3(3) . . ? C3 C2 C1 106.9(4) . . ? C3 C2 C7 127.0(4) . . ? C1 C2 C7 125.9(4) . . ? C3 C2 Ti1 73.3(2) . . ? C1 C2 Ti1 69.3(2) . . ? C7 C2 Ti1 125.1(3) . . ? C2 C3 C4 108.9(4) . . ? C2 C3 C8 125.4(4) . . ? C4 C3 C8 125.6(4) . . ? C2 C3 Ti1 73.5(2) . . ? C4 C3 Ti1 69.1(2) . . ? C8 C3 Ti1 125.6(3) . . ? C3 C4 C5 107.4(4) . . ? C3 C4 C9 125.5(4) . . ? C5 C4 C9 126.7(4) . . ? C3 C4 Ti1 76.7(2) . . ? C5 C4 Ti1 71.4(2) . . ? C9 C4 Ti1 123.6(3) . . ? C1 C5 C4 108.2(4) . . ? C1 C5 C10 125.2(4) . . ? C4 C5 C10 126.4(4) . . ? C1 C5 Ti1 74.2(2) . . ? C4 C5 Ti1 73.4(2) . . ? C10 C5 Ti1 122.1(3) . . ? C14 C11 C12 110.6(4) . . ? C14 C11 C13 108.8(3) . . ? C12 C11 C13 107.6(3) . . ? C14 C11 P1 113.1(3) . . ? C12 C11 P1 110.1(3) . . ? C13 C11 P1 106.4(3) . . ? C18 C15 C16 108.6(3) . . ? C18 C15 C17 109.7(3) . . ? C16 C15 C17 108.6(3) . . ? C18 C15 P1 106.4(3) . . ? C16 C15 P1 111.1(3) . . ? C17 C15 P1 112.4(3) . . ? C23 C19 C20 106.6(3) . . ? C23 C19 P1 119.9(3) . . ? C20 C19 P1 130.4(3) . . ? C23 C19 Fe1 69.8(2) . . ? C20 C19 Fe1 69.3(2) . . ? P1 C19 Fe1 140.8(2) . . ? C21 C20 C19 108.6(4) . . ? C21 C20 Fe1 70.1(2) . . ? C19 C20 Fe1 69.9(2) . . ? C22 C21 C20 108.0(4) . . ? C22 C21 Fe1 69.8(2) . . ? C20 C21 Fe1 69.7(2) . . ? C21 C22 C23 108.7(4) . . ? C21 C22 Fe1 70.2(2) . . ? C23 C22 Fe1 70.3(2) . . ? C22 C23 C19 108.0(4) . . ? C22 C23 Fe1 69.5(2) . . ? C19 C23 Fe1 69.5(2) . . ? Cl4 C24 Cl5 109.8(3) . . ? Cl4 C24 Cl3 110.5(3) . . ? Cl5 C24 Cl3 110.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.775 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.093 #===end