Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Michael Hill' 'David Evans' 'Peter B. Hitchcock' _publ_contact_author_name 'Dr Michael Hill' _publ_contact_author_address ; Department of Chemistry University of Sussex Falmer Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.S.HILL@SUSSEX.AC.UK _publ_requested_journal 'Dalton Trans.' _publ_section_title ; Tuning low-coordinate metal environments: high spin d5-d7 complexes supported by bis(phosphinimino)methyl ligation ; data_sep1301 _database_code_CSD 191080 _audit_creation_date 2001-09-17T16:41:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[(MesNPPh2CHPPh2NMes)FeCl2Li(thf)(ET2O)]' ; _chemical_formula_moiety 'C51 H61 Cl2 Fe Li N2 O2 P2' _chemical_formula_sum 'C51 H61 Cl2 Fe Li N2 O2 P2' _chemical_formula_weight 929.65 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8140(12) _cell_length_b 13.1172(7) _cell_length_c 16.2526(16) _cell_angle_alpha 91.262(6) _cell_angle_beta 101.066(4) _cell_angle_gamma 117.249(5) _cell_volume 2364.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11086 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.976 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 12078 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_unetI/netI 0.0888 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.7 _diffrn_reflns_theta_max 21.95 _diffrn_reflns_theta_full 21.95 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 5716 _reflns_number_gt 4151 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+2.4476P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 5716 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.291 _refine_diff_density_min -0.31 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.53537(5) 0.35940(5) 0.23942(4) 0.02415(19) Uani 1 1 d . . . Li Li 0.4484(7) 0.5162(6) 0.3312(5) 0.041(2) Uani 1 1 d . . . Cl1 Cl 0.42605(11) 0.45794(9) 0.18627(8) 0.0361(3) Uani 1 1 d . . . Cl2 Cl 0.56521(10) 0.42230(9) 0.38370(7) 0.0338(3) Uani 1 1 d . . . P1 P 0.44733(10) 0.10796(9) 0.13788(7) 0.0224(3) Uani 1 1 d . . . P2 P 0.71027(10) 0.29138(9) 0.19194(7) 0.0216(3) Uani 1 1 d . . . O1 O 0.3070(3) 0.4614(3) 0.3766(2) 0.0451(9) Uani 1 1 d . . . O2 O 0.5413(3) 0.6826(2) 0.3516(2) 0.0438(9) Uani 1 1 d . . . N1 N 0.6991(3) 0.4075(2) 0.2141(2) 0.0225(9) Uani 1 1 d . . . N2 N 0.4294(3) 0.1846(3) 0.2094(2) 0.0228(9) Uani 1 1 d . . . C1 C 0.5904(4) 0.1801(3) 0.1228(3) 0.0241(11) Uani 1 1 d . . . H1 H 0.6051 0.157 0.0723 0.029 Uiso 1 1 calc R . . C2 C 0.4034(4) -0.0412(3) 0.1609(3) 0.0235(10) Uani 1 1 d . . . C3 C 0.4702(4) -0.0924(3) 0.1395(3) 0.0299(12) Uani 1 1 d . . . H3 H 0.543 -0.0467 0.1223 0.036 Uiso 1 1 calc R . . C4 C 0.4315(4) -0.2097(3) 0.1430(3) 0.0310(12) Uani 1 1 d . . . H4 H 0.4781 -0.2433 0.1281 0.037 Uiso 1 1 calc R . . C5 C 0.3268(4) -0.2774(4) 0.1679(3) 0.0353(12) Uani 1 1 d . . . H5 H 0.3009 -0.3575 0.1701 0.042 Uiso 1 1 calc R . . C6 C 0.2593(4) -0.2279(3) 0.1896(3) 0.0328(12) Uani 1 1 d . . . H6 H 0.1875 -0.2741 0.2078 0.039 Uiso 1 1 calc R . . C7 C 0.2955(4) -0.1114(3) 0.1849(3) 0.0276(11) Uani 1 1 d . . . H7 H 0.247 -0.079 0.1981 0.033 Uiso 1 1 calc R . . C8 C 0.3483(4) 0.0791(3) 0.0331(3) 0.0211(10) Uani 1 1 d . . . C9 C 0.3577(4) 0.1747(3) -0.0082(3) 0.0258(11) Uani 1 1 d . . . H9 H 0.412 0.2504 0.0197 0.031 Uiso 1 1 calc R . . C10 C 0.2899(4) 0.1612(4) -0.0884(3) 0.0292(11) Uani 1 1 d . . . H10 H 0.2993 0.227 -0.1159 0.035 Uiso 1 1 calc R . . C11 C 0.2080(4) 0.0513(4) -0.1286(3) 0.0320(12) Uani 1 1 d . . . H11 H 0.1613 0.0414 -0.184 0.038 Uiso 1 1 calc R . . C12 C 0.1946(4) -0.0434(4) -0.0882(3) 0.0334(12) Uani 1 1 d . . . H12 H 0.1367 -0.1186 -0.1153 0.04 Uiso 1 1 calc R . . C13 C 0.2648(4) -0.0301(3) -0.0082(3) 0.0286(11) Uani 1 1 d . . . H13 H 0.2556 -0.0965 0.0186 0.034 Uiso 1 1 calc R . . C14 C 0.3333(4) 0.1353(3) 0.2532(3) 0.0225(10) Uani 1 1 d . . . C15 C 0.3554(4) 0.0981(3) 0.3321(3) 0.0235(11) Uani 1 1 d . . . C16 C 0.2640(4) 0.0533(3) 0.3767(3) 0.0297(11) Uani 1 1 d . . . H16 H 0.2792 0.0267 0.4293 0.036 Uiso 1 1 calc R . . C17 C 0.1524(4) 0.0464(3) 0.3463(3) 0.0315(12) Uani 1 1 d . . . C18 C 0.1332(4) 0.0850(3) 0.2696(3) 0.0298(12) Uani 1 1 d . . . H18 H 0.0572 0.0818 0.2486 0.036 Uiso 1 1 calc R . . C19 C 0.2198(4) 0.1285(3) 0.2211(3) 0.0243(11) Uani 1 1 d . . . C20 C 0.4759(4) 0.1048(4) 0.3691(3) 0.0329(12) Uani 1 1 d . . . H20A H 0.5352 0.1852 0.3906 0.049 Uiso 1 1 calc R . . H20B H 0.5023 0.0761 0.3253 0.049 Uiso 1 1 calc R . . H20C H 0.4685 0.0572 0.4155 0.049 Uiso 1 1 calc R . . C21 C 0.0557(4) -0.0001(4) 0.3966(4) 0.0528(15) Uani 1 1 d . . . H21A H -0.0069 0.0219 0.3745 0.079 Uiso 1 1 calc R . . H21B H 0.0915 0.0322 0.4561 0.079 Uiso 1 1 calc R . . H21C H 0.0198 -0.0846 0.3916 0.079 Uiso 1 1 calc R . . C22 C 0.1887(4) 0.1649(4) 0.1366(3) 0.0337(12) Uani 1 1 d . . . H22A H 0.2582 0.2355 0.1287 0.051 Uiso 1 1 calc R . . H22B H 0.12 0.1798 0.1345 0.051 Uiso 1 1 calc R . . H22C H 0.1676 0.1032 0.0917 0.051 Uiso 1 1 calc R . . C23 C 0.8432(4) 0.3285(3) 0.1501(3) 0.0225(11) Uani 1 1 d . . . C24 C 0.9535(4) 0.3555(3) 0.2041(3) 0.0314(12) Uani 1 1 d . . . H24 H 0.9587 0.3525 0.263 0.038 Uiso 1 1 calc R . . C25 C 1.0552(4) 0.3866(4) 0.1726(4) 0.0422(13) Uani 1 1 d . . . H25 H 1.1299 0.4046 0.2098 0.051 Uiso 1 1 calc R . . C26 C 1.0488(5) 0.3917(4) 0.0876(4) 0.0407(13) Uani 1 1 d . . . H26 H 1.1191 0.4133 0.0662 0.049 Uiso 1 1 calc R . . C27 C 0.9408(4) 0.3655(3) 0.0332(3) 0.0346(12) Uani 1 1 d . . . H27 H 0.9365 0.3685 -0.0256 0.041 Uiso 1 1 calc R . . C28 C 0.8386(4) 0.3348(3) 0.0643(3) 0.0289(11) Uani 1 1 d . . . H28 H 0.7645 0.3178 0.0267 0.035 Uiso 1 1 calc R . . C29 C 0.7433(4) 0.2412(3) 0.2923(3) 0.0225(10) Uani 1 1 d . . . C30 C 0.7471(4) 0.1360(3) 0.2915(3) 0.0326(12) Uani 1 1 d . . . H30 H 0.7257 0.0893 0.2394 0.039 Uiso 1 1 calc R . . C31 C 0.7821(4) 0.1000(4) 0.3667(4) 0.0465(14) Uani 1 1 d . . . H31 H 0.7863 0.0296 0.3658 0.056 Uiso 1 1 calc R . . C32 C 0.8108(4) 0.1662(4) 0.4427(4) 0.0450(14) Uani 1 1 d . . . H32 H 0.8348 0.1412 0.494 0.054 Uiso 1 1 calc R . . C33 C 0.8048(4) 0.2681(4) 0.4444(3) 0.0385(13) Uani 1 1 d . . . H33 H 0.824 0.3132 0.4969 0.046 Uiso 1 1 calc R . . C34 C 0.7706(4) 0.3053(4) 0.3694(3) 0.0296(12) Uani 1 1 d . . . H34 H 0.7658 0.3755 0.3711 0.036 Uiso 1 1 calc R . . C35 C 0.7706(4) 0.5152(3) 0.1826(3) 0.0227(11) Uani 1 1 d . . . C36 C 0.7334(4) 0.5352(3) 0.1003(3) 0.0213(10) Uani 1 1 d . . . C37 C 0.8047(4) 0.6395(3) 0.0725(3) 0.0258(11) Uani 1 1 d . . . H37 H 0.7791 0.6521 0.0166 0.031 Uiso 1 1 calc R . . C38 C 0.9105(4) 0.7248(3) 0.1226(3) 0.0273(11) Uani 1 1 d . . . C39 C 0.9434(4) 0.7053(3) 0.2050(3) 0.0318(12) Uani 1 1 d . . . H39 H 1.0143 0.7641 0.2414 0.038 Uiso 1 1 calc R . . C40 C 0.8764(4) 0.6027(3) 0.2364(3) 0.0263(11) Uani 1 1 d . . . C41 C 0.6193(4) 0.4480(3) 0.0416(3) 0.0301(11) Uani 1 1 d . . . H41A H 0.5499 0.4433 0.0616 0.045 Uiso 1 1 calc R . . H41B H 0.6169 0.3723 0.0401 0.045 Uiso 1 1 calc R . . H41C H 0.6163 0.4715 -0.0153 0.045 Uiso 1 1 calc R . . C42 C 0.9861(4) 0.8354(3) 0.0891(3) 0.0360(12) Uani 1 1 d . . . H42A H 1.0406 0.8238 0.0598 0.054 Uiso 1 1 calc R . . H42B H 1.0334 0.8975 0.1363 0.054 Uiso 1 1 calc R . . H42C H 0.9332 0.8565 0.0496 0.054 Uiso 1 1 calc R . . C43 C 0.9185(4) 0.5891(4) 0.3260(3) 0.0418(13) Uani 1 1 d . . . H43A H 0.9408 0.5269 0.3268 0.063 Uiso 1 1 calc R . . H43B H 0.8535 0.5699 0.3559 0.063 Uiso 1 1 calc R . . H43C H 0.9887 0.6616 0.354 0.063 Uiso 1 1 calc R . . C44 C 0.2407(4) 0.5180(4) 0.3984(3) 0.0448(14) Uani 1 1 d . . . H44A H 0.2029 0.5389 0.3471 0.054 Uiso 1 1 calc R . . H44B H 0.295 0.5893 0.4381 0.054 Uiso 1 1 calc R . . C45 C 0.1449(5) 0.4325(4) 0.4395(4) 0.0553(15) Uani 1 1 d . . . H45A H 0.1665 0.4545 0.5014 0.066 Uiso 1 1 calc R . . H45B H 0.0656 0.4282 0.4161 0.066 Uiso 1 1 calc R . . C46 C 0.1427(5) 0.3189(4) 0.4184(4) 0.0587(16) Uani 1 1 d . . . H46A H 0.1192 0.2682 0.463 0.07 Uiso 1 1 calc R . . H46B H 0.0863 0.278 0.3636 0.07 Uiso 1 1 calc R . . C47 C 0.2697(5) 0.3549(4) 0.4140(4) 0.0545(16) Uani 1 1 d . . . H47A H 0.3209 0.3677 0.4712 0.065 Uiso 1 1 calc R . . H47B H 0.2744 0.2955 0.3785 0.065 Uiso 1 1 calc R . . C48 C 0.5469(5) 0.7557(4) 0.4204(4) 0.0526(15) Uani 1 1 d . . . H48A H 0.6324 0.8093 0.447 0.063 Uiso 1 1 calc R . . H48B H 0.5102 0.7078 0.4634 0.063 Uiso 1 1 calc R . . C49 C 0.4819(6) 0.8251(5) 0.3921(4) 0.075(2) Uani 1 1 d . . . H49A H 0.4875 0.8739 0.441 0.113 Uiso 1 1 calc R . . H49B H 0.3969 0.7722 0.3666 0.113 Uiso 1 1 calc R . . H49C H 0.5192 0.8739 0.3504 0.113 Uiso 1 1 calc R . . C50 C 0.6285(5) 0.7398(4) 0.3020(4) 0.0583(16) Uani 1 1 d . . . H50A H 0.6372 0.8181 0.2964 0.07 Uiso 1 1 calc R . . H50B H 0.5982 0.6964 0.2446 0.07 Uiso 1 1 calc R . . C51 C 0.7467(5) 0.7497(5) 0.3384(5) 0.085(2) Uani 1 1 d . . . H51A H 0.8021 0.7894 0.302 0.128 Uiso 1 1 calc R . . H51B H 0.7392 0.6724 0.3428 0.128 Uiso 1 1 calc R . . H51C H 0.7781 0.7941 0.3947 0.128 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 Fe 0.0242(4) 0.0213(3) 0.0260(4) 0.0011(3) 0.0077(3) 0.0092(3) Li 0.050(5) 0.036(4) 0.042(6) -0.001(4) 0.013(5) 0.023(4) Cl1 0.0440(7) 0.0362(6) 0.0334(8) 0.0035(5) 0.0063(6) 0.0244(6) Cl2 0.0403(7) 0.0370(6) 0.0272(7) 0.0004(5) 0.0084(6) 0.0206(6) P1 0.0222(6) 0.0208(6) 0.0231(7) 0.0005(5) 0.0061(6) 0.0090(5) P2 0.0209(6) 0.0218(6) 0.0224(7) 0.0021(5) 0.0060(6) 0.0099(5) O1 0.055(2) 0.0400(19) 0.053(2) 0.0092(17) 0.031(2) 0.0266(17) O2 0.050(2) 0.0318(18) 0.054(3) 0.0038(17) 0.023(2) 0.0185(16) N1 0.025(2) 0.0188(19) 0.025(2) 0.0037(16) 0.0098(18) 0.0106(16) N2 0.027(2) 0.0236(19) 0.022(2) 0.0044(16) 0.0132(18) 0.0121(16) C1 0.024(3) 0.023(2) 0.024(3) -0.0025(19) 0.008(2) 0.0097(19) C2 0.027(3) 0.022(2) 0.020(3) 0.0008(19) 0.004(2) 0.011(2) C3 0.027(3) 0.026(3) 0.034(3) 0.002(2) 0.007(2) 0.010(2) C4 0.036(3) 0.027(3) 0.034(3) 0.001(2) 0.007(2) 0.018(2) C5 0.040(3) 0.023(3) 0.040(3) 0.005(2) 0.007(3) 0.014(2) C6 0.030(3) 0.025(3) 0.039(3) 0.006(2) 0.015(2) 0.007(2) C7 0.029(3) 0.025(3) 0.028(3) 0.001(2) 0.008(2) 0.012(2) C8 0.018(2) 0.027(2) 0.021(3) -0.002(2) 0.008(2) 0.012(2) C9 0.023(2) 0.022(2) 0.032(3) 0.000(2) 0.012(2) 0.0078(19) C10 0.027(3) 0.034(3) 0.030(3) 0.002(2) 0.005(3) 0.018(2) C11 0.026(3) 0.049(3) 0.025(3) -0.001(2) 0.005(2) 0.021(2) C12 0.027(3) 0.030(3) 0.035(3) -0.006(2) -0.001(3) 0.010(2) C13 0.028(3) 0.027(3) 0.035(3) 0.003(2) 0.012(3) 0.014(2) C14 0.023(3) 0.019(2) 0.024(3) -0.0016(19) 0.009(2) 0.0075(19) C15 0.021(3) 0.023(2) 0.025(3) 0.002(2) 0.007(2) 0.0088(19) C16 0.035(3) 0.026(2) 0.027(3) 0.005(2) 0.012(3) 0.011(2) C17 0.032(3) 0.030(3) 0.031(3) 0.002(2) 0.014(3) 0.011(2) C18 0.017(2) 0.032(3) 0.035(3) -0.002(2) 0.006(2) 0.007(2) C19 0.024(3) 0.018(2) 0.027(3) -0.0015(19) 0.004(2) 0.0071(19) C20 0.034(3) 0.039(3) 0.025(3) 0.009(2) 0.009(2) 0.016(2) C21 0.037(3) 0.070(4) 0.054(4) 0.021(3) 0.026(3) 0.022(3) C22 0.027(3) 0.035(3) 0.040(3) 0.002(2) 0.004(2) 0.017(2) C23 0.023(3) 0.018(2) 0.027(3) -0.0001(19) 0.011(2) 0.0079(19) C24 0.030(3) 0.035(3) 0.025(3) -0.002(2) 0.008(3) 0.011(2) C25 0.022(3) 0.051(3) 0.045(4) -0.007(3) 0.006(3) 0.011(2) C26 0.036(3) 0.034(3) 0.048(4) -0.003(2) 0.022(3) 0.008(2) C27 0.041(3) 0.031(3) 0.032(3) 0.005(2) 0.015(3) 0.014(2) C28 0.032(3) 0.023(2) 0.032(3) 0.004(2) 0.010(2) 0.012(2) C29 0.020(2) 0.025(2) 0.022(3) 0.007(2) 0.009(2) 0.0085(19) C30 0.034(3) 0.028(3) 0.038(3) 0.004(2) 0.009(3) 0.016(2) C31 0.046(3) 0.038(3) 0.063(4) 0.021(3) 0.014(3) 0.024(3) C32 0.037(3) 0.052(3) 0.042(4) 0.022(3) 0.006(3) 0.018(3) C33 0.035(3) 0.042(3) 0.035(3) 0.009(2) 0.008(3) 0.015(2) C34 0.026(3) 0.030(3) 0.030(3) 0.011(2) 0.009(2) 0.011(2) C35 0.022(2) 0.021(2) 0.028(3) 0.002(2) 0.009(2) 0.011(2) C36 0.021(2) 0.021(2) 0.022(3) 0.0017(19) 0.007(2) 0.0095(19) C37 0.033(3) 0.030(3) 0.022(3) 0.006(2) 0.010(2) 0.020(2) C38 0.025(3) 0.029(3) 0.033(3) 0.006(2) 0.013(2) 0.014(2) C39 0.027(3) 0.022(3) 0.037(3) -0.004(2) 0.002(2) 0.006(2) C40 0.028(3) 0.024(2) 0.025(3) 0.000(2) 0.004(2) 0.011(2) C41 0.037(3) 0.028(2) 0.026(3) 0.010(2) 0.008(2) 0.015(2) C42 0.032(3) 0.028(3) 0.044(3) 0.006(2) 0.013(3) 0.009(2) C43 0.038(3) 0.033(3) 0.038(4) 0.000(2) -0.006(3) 0.008(2) C44 0.050(3) 0.046(3) 0.044(4) -0.002(3) 0.014(3) 0.027(3) C45 0.047(4) 0.069(4) 0.051(4) -0.001(3) 0.011(3) 0.028(3) C46 0.042(4) 0.056(4) 0.071(5) 0.016(3) 0.019(3) 0.014(3) C47 0.057(4) 0.038(3) 0.074(5) 0.015(3) 0.023(3) 0.023(3) C48 0.063(4) 0.044(3) 0.051(4) -0.008(3) 0.009(3) 0.027(3) C49 0.120(6) 0.071(4) 0.058(5) 0.011(3) 0.017(4) 0.065(4) C50 0.062(4) 0.049(3) 0.063(4) 0.014(3) 0.029(4) 0.018(3) C51 0.054(4) 0.086(5) 0.121(7) 0.029(4) 0.030(4) 0.031(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.025(3) . ? Fe N2 2.046(3) . ? Fe Cl2 2.3680(13) . ? Fe Cl1 2.3711(12) . ? Fe Li 3.209(8) . ? Li O1 1.921(9) . ? Li O2 1.931(8) . ? Li Cl1 2.382(9) . ? Li Cl2 2.393(8) . ? P1 N2 1.636(3) . ? P1 C1 1.706(4) . ? P1 C8 1.832(4) . ? P1 C2 1.842(4) . ? P2 N1 1.632(3) . ? P2 C1 1.722(4) . ? P2 C23 1.817(4) . ? P2 C29 1.820(4) . ? O1 C44 1.442(5) . ? O1 C47 1.445(5) . ? O2 C48 1.426(6) . ? O2 C50 1.436(6) . ? N1 C35 1.457(5) . ? N2 C14 1.438(5) . ? C2 C3 1.391(6) . ? C2 C7 1.403(6) . ? C3 C4 1.390(5) . ? C4 C5 1.373(6) . ? C5 C6 1.384(6) . ? C6 C7 1.387(5) . ? C8 C13 1.387(5) . ? C8 C9 1.404(6) . ? C9 C10 1.377(6) . ? C10 C11 1.385(6) . ? C11 C12 1.374(6) . ? C12 C13 1.390(6) . ? C14 C15 1.406(6) . ? C14 C19 1.408(6) . ? C15 C16 1.398(6) . ? C15 C20 1.507(6) . ? C16 C17 1.382(6) . ? C17 C18 1.376(6) . ? C17 C21 1.514(6) . ? C18 C19 1.400(6) . ? C19 C22 1.505(6) . ? C23 C28 1.390(6) . ? C23 C24 1.394(6) . ? C24 C25 1.381(6) . ? C25 C26 1.373(7) . ? C26 C27 1.377(6) . ? C27 C28 1.383(6) . ? C29 C34 1.385(6) . ? C29 C30 1.402(5) . ? C30 C31 1.389(7) . ? C31 C32 1.378(7) . ? C32 C33 1.374(6) . ? C33 C34 1.390(6) . ? C35 C36 1.404(6) . ? C35 C40 1.412(6) . ? C36 C37 1.397(5) . ? C36 C41 1.497(6) . ? C37 C38 1.378(6) . ? C38 C39 1.391(6) . ? C38 C42 1.513(6) . ? C39 C40 1.396(6) . ? C40 C43 1.498(6) . ? C44 C45 1.515(7) . ? C45 C46 1.508(7) . ? C46 C47 1.489(7) . ? C48 C49 1.516(7) . ? C50 C51 1.461(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe N2 110.11(13) . . ? N1 Fe Cl2 108.05(10) . . ? N2 Fe Cl2 112.69(10) . . ? N1 Fe Cl1 119.23(10) . . ? N2 Fe Cl1 110.41(10) . . ? Cl2 Fe Cl1 95.61(4) . . ? N1 Fe Li 127.99(17) . . ? N2 Fe Li 121.61(17) . . ? Cl2 Fe Li 47.97(16) . . ? Cl1 Fe Li 47.68(16) . . ? O1 Li O2 111.5(4) . . ? O1 Li Cl1 118.8(4) . . ? O2 Li Cl1 107.9(4) . . ? O1 Li Cl2 110.5(4) . . ? O2 Li Cl2 112.5(4) . . ? Cl1 Li Cl2 94.7(3) . . ? O1 Li Fe 126.3(3) . . ? O2 Li Fe 122.1(4) . . ? Cl1 Li Fe 47.40(14) . . ? Cl2 Li Fe 47.30(14) . . ? Fe Cl1 Li 84.92(19) . . ? Fe Cl2 Li 84.7(2) . . ? N2 P1 C1 109.63(19) . . ? N2 P1 C8 115.04(18) . . ? C1 P1 C8 105.4(2) . . ? N2 P1 C2 112.77(18) . . ? C1 P1 C2 113.77(19) . . ? C8 P1 C2 99.88(18) . . ? N1 P2 C1 117.72(19) . . ? N1 P2 C23 110.13(17) . . ? C1 P2 C23 107.2(2) . . ? N1 P2 C29 106.60(19) . . ? C1 P2 C29 110.41(19) . . ? C23 P2 C29 103.9(2) . . ? C44 O1 C47 108.5(4) . . ? C44 O1 Li 131.7(4) . . ? C47 O1 Li 118.3(4) . . ? C48 O2 C50 114.4(4) . . ? C48 O2 Li 126.4(4) . . ? C50 O2 Li 118.4(4) . . ? C35 N1 P2 120.9(3) . . ? C35 N1 Fe 125.2(2) . . ? P2 N1 Fe 108.66(16) . . ? C14 N2 P1 122.6(3) . . ? C14 N2 Fe 114.3(2) . . ? P1 N2 Fe 123.06(18) . . ? P1 C1 P2 125.2(3) . . ? C3 C2 C7 118.2(4) . . ? C3 C2 P1 117.6(3) . . ? C7 C2 P1 123.3(3) . . ? C2 C3 C4 120.7(4) . . ? C5 C4 C3 120.7(4) . . ? C4 C5 C6 119.4(4) . . ? C5 C6 C7 120.6(4) . . ? C6 C7 C2 120.4(4) . . ? C13 C8 C9 117.8(4) . . ? C13 C8 P1 124.9(3) . . ? C9 C8 P1 117.4(3) . . ? C10 C9 C8 121.4(4) . . ? C9 C10 C11 119.7(4) . . ? C12 C11 C10 119.8(4) . . ? C11 C12 C13 120.6(4) . . ? C8 C13 C12 120.6(4) . . ? C15 C14 C19 119.3(4) . . ? C15 C14 N2 119.0(4) . . ? C19 C14 N2 121.7(4) . . ? C16 C15 C14 119.6(4) . . ? C16 C15 C20 119.4(4) . . ? C14 C15 C20 121.0(4) . . ? C17 C16 C15 121.9(4) . . ? C18 C17 C16 117.6(4) . . ? C18 C17 C21 121.5(4) . . ? C16 C17 C21 121.0(4) . . ? C17 C18 C19 123.4(4) . . ? C18 C19 C14 118.2(4) . . ? C18 C19 C22 119.3(4) . . ? C14 C19 C22 122.4(4) . . ? C28 C23 C24 118.5(4) . . ? C28 C23 P2 121.0(3) . . ? C24 C23 P2 120.5(3) . . ? C25 C24 C23 120.5(5) . . ? C26 C25 C24 120.2(5) . . ? C25 C26 C27 120.2(5) . . ? C26 C27 C28 120.0(5) . . ? C27 C28 C23 120.6(4) . . ? C34 C29 C30 118.6(4) . . ? C34 C29 P2 122.6(3) . . ? C30 C29 P2 118.7(3) . . ? C31 C30 C29 120.2(5) . . ? C32 C31 C30 120.2(4) . . ? C33 C32 C31 120.2(5) . . ? C32 C33 C34 120.1(5) . . ? C29 C34 C33 120.7(4) . . ? C36 C35 C40 119.3(4) . . ? C36 C35 N1 120.9(4) . . ? C40 C35 N1 119.9(4) . . ? C37 C36 C35 119.1(4) . . ? C37 C36 C41 119.1(4) . . ? C35 C36 C41 121.8(4) . . ? C38 C37 C36 122.9(4) . . ? C37 C38 C39 117.1(4) . . ? C37 C38 C42 121.1(4) . . ? C39 C38 C42 121.8(4) . . ? C38 C39 C40 122.6(4) . . ? C39 C40 C35 118.9(4) . . ? C39 C40 C43 119.0(4) . . ? C35 C40 C43 122.1(4) . . ? O1 C44 C45 106.4(4) . . ? C46 C45 C44 104.2(4) . . ? C47 C46 C45 102.8(4) . . ? O1 C47 C46 104.6(4) . . ? O2 C48 C49 111.9(5) . . ? O2 C50 C51 113.2(5) . . ? #===END data_apr502 _database_code_CSD 198768 _audit_creation_date 2002-04-16T14:03:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Mn{N(SiMe3)2}{MesNPPh2CHPPh2NMes}] _chemical_formula_moiety 'C49 H61 Mn N3 P2 Si2' _chemical_formula_sum 'C49 H61 Mn N3 P2 Si2' _chemical_formula_weight 865.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 23.9011(4) _cell_length_b 15.5577(3) _cell_length_c 12.6739(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4712.74(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39974 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.908 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_number 30367 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 24.69 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 7304 _reflns_number_gt 6402 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; H on C1 was freely refined. Methyl H atoms riding with torsion angle refined. Para-methyl H atoms disordered (AFIX 123) Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+1.9947P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7304 _refine_ls_number_parameters 528 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(14) _refine_diff_density_max 0.199 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.358030(16) 0.21164(3) 0.41951(3) 0.02180(11) Uani 1 1 d . . . P1 P 0.43011(3) 0.33581(5) 0.53371(5) 0.02127(17) Uani 1 1 d . . . P2 P 0.36992(3) 0.38479(5) 0.32202(6) 0.02304(18) Uani 1 1 d . . . Si1 Si 0.29104(3) 0.04696(6) 0.47941(7) 0.0298(2) Uani 1 1 d . . . Si2 Si 0.38112(3) 0.02379(6) 0.31535(6) 0.0306(2) Uani 1 1 d . . . N1 N 0.39049(9) 0.25538(15) 0.56475(16) 0.0210(5) Uani 1 1 d . . . N2 N 0.32029(9) 0.31634(16) 0.33894(17) 0.0229(5) Uani 1 1 d . . . N3 N 0.34207(9) 0.08590(16) 0.39750(17) 0.0241(6) Uani 1 1 d . . . C1 C 0.42476(12) 0.3497(2) 0.3982(2) 0.0269(7) Uani 1 1 d . . . H1 H 0.4586(17) 0.364(3) 0.371(3) 0.076(14) Uiso 1 1 d . . . C2 C 0.41324(12) 0.4317(2) 0.6099(2) 0.0257(7) Uani 1 1 d . . . C3 C 0.35752(12) 0.4584(2) 0.6135(2) 0.0297(7) Uani 1 1 d . . . H3 H 0.3298 0.4259 0.5776 0.036 Uiso 1 1 calc R . . C4 C 0.34208(14) 0.5315(2) 0.6684(3) 0.0399(9) Uani 1 1 d . . . H4 H 0.304 0.5488 0.6696 0.048 Uiso 1 1 calc R . . C5 C 0.38117(16) 0.5787(2) 0.7206(3) 0.0479(10) Uani 1 1 d . . . H5 H 0.3704 0.6278 0.7602 0.058 Uiso 1 1 calc R . . C6 C 0.43692(16) 0.5544(3) 0.7155(3) 0.0548(11) Uani 1 1 d . . . H6 H 0.4644 0.588 0.7507 0.066 Uiso 1 1 calc R . . C7 C 0.45316(14) 0.4824(2) 0.6601(2) 0.0390(9) Uani 1 1 d . . . H7 H 0.4916 0.4674 0.6561 0.047 Uiso 1 1 calc R . . C8 C 0.50287(11) 0.3160(2) 0.5652(2) 0.0243(7) Uani 1 1 d . . . C9 C 0.54503(11) 0.3089(2) 0.4900(2) 0.0333(8) Uani 1 1 d . . . H9 H 0.5368 0.3193 0.4178 0.04 Uiso 1 1 calc R . . C10 C 0.59879(13) 0.2868(2) 0.5193(3) 0.0444(9) Uani 1 1 d . . . H10 H 0.6273 0.2836 0.4673 0.053 Uiso 1 1 calc R . . C11 C 0.61153(14) 0.2694(3) 0.6231(3) 0.0479(10) Uani 1 1 d . . . H11 H 0.6485 0.2534 0.6424 0.057 Uiso 1 1 calc R . . C12 C 0.57063(13) 0.2755(2) 0.6979(3) 0.0416(9) Uani 1 1 d . . . H12 H 0.5793 0.2632 0.7695 0.05 Uiso 1 1 calc R . . C13 C 0.51638(13) 0.2994(2) 0.6706(2) 0.0328(8) Uani 1 1 d . . . H13 H 0.4885 0.3045 0.7237 0.039 Uiso 1 1 calc R . . C14 C 0.34867(12) 0.4951(2) 0.3468(2) 0.0265(7) Uani 1 1 d . . . C15 C 0.29642(12) 0.5262(2) 0.3150(3) 0.0391(8) Uani 1 1 d . . . H15 H 0.2712 0.4887 0.2799 0.047 Uiso 1 1 calc R . . C16 C 0.28075(15) 0.6096(2) 0.3334(3) 0.0496(9) Uani 1 1 d . . . H16 H 0.2453 0.6297 0.3103 0.059 Uiso 1 1 calc R . . C17 C 0.31664(19) 0.6640(3) 0.3854(3) 0.0534(11) Uani 1 1 d . . . H17 H 0.3056 0.7215 0.3995 0.064 Uiso 1 1 calc R . . C18 C 0.36811(18) 0.6359(2) 0.4169(3) 0.0527(10) Uani 1 1 d . . . H18 H 0.3926 0.6741 0.4527 0.063 Uiso 1 1 calc R . . C19 C 0.38504(15) 0.5519(2) 0.3971(2) 0.0387(8) Uani 1 1 d . . . H19 H 0.4213 0.5332 0.4178 0.046 Uiso 1 1 calc R . . C20 C 0.39837(12) 0.3909(2) 0.1881(2) 0.0261(7) Uani 1 1 d . . . C21 C 0.43211(13) 0.3243(2) 0.1509(2) 0.0374(8) Uani 1 1 d . . . H21 H 0.4419 0.2785 0.1968 0.045 Uiso 1 1 calc R . . C22 C 0.45144(14) 0.3240(3) 0.0480(3) 0.0465(10) Uani 1 1 d . . . H22 H 0.4743 0.2781 0.0238 0.056 Uiso 1 1 calc R . . C23 C 0.43763(15) 0.3902(3) -0.0195(3) 0.0493(10) Uani 1 1 d . . . H23 H 0.4506 0.3898 -0.0903 0.059 Uiso 1 1 calc R . . C24 C 0.40511(15) 0.4567(3) 0.0162(2) 0.0469(10) Uani 1 1 d . . . H24 H 0.3958 0.5024 -0.0302 0.056 Uiso 1 1 calc R . . C25 C 0.38556(13) 0.4578(2) 0.1200(2) 0.0355(8) Uani 1 1 d . . . H25 H 0.3634 0.5046 0.144 0.043 Uiso 1 1 calc R . . C26 C 0.39638(11) 0.2085(2) 0.6623(2) 0.0222(7) Uani 1 1 d . . . C27 C 0.43393(12) 0.1391(2) 0.6673(2) 0.0269(7) Uani 1 1 d . . . C28 C 0.44015(13) 0.0946(2) 0.7615(2) 0.0357(8) Uani 1 1 d . . . H28 H 0.4659 0.0482 0.7642 0.043 Uiso 1 1 calc R . . C29 C 0.41056(14) 0.1149(3) 0.8509(2) 0.0404(9) Uani 1 1 d . . . C30 C 0.37215(13) 0.1810(2) 0.8439(2) 0.0360(8) Uani 1 1 d . . . H30 H 0.3506 0.1952 0.9044 0.043 Uiso 1 1 calc R . . C31 C 0.36381(12) 0.2277(2) 0.7514(2) 0.0270(7) Uani 1 1 d . . . C32 C 0.46699(13) 0.1092(2) 0.5727(2) 0.0350(8) Uani 1 1 d . . . H32C H 0.4875 0.1579 0.5426 0.052 Uiso 1 1 calc R . . H32B H 0.4414 0.0857 0.5196 0.052 Uiso 1 1 calc R . . H32A H 0.4935 0.0646 0.5945 0.052 Uiso 1 1 calc R . . C33 C 0.41815(18) 0.0659(3) 0.9537(3) 0.0720(13) Uani 1 1 d . . . H33F H 0.41 0.0049 0.9421 0.108 Uiso 0.5 1 calc PR . . H33E H 0.3925 0.0889 1.0071 0.108 Uiso 0.5 1 calc PR . . H33D H 0.4568 0.0722 0.9783 0.108 Uiso 0.5 1 calc PR . . H33C H 0.4296 0.1058 1.0095 0.108 Uiso 0.5 1 calc PR . . H33B H 0.447 0.0218 0.9445 0.108 Uiso 0.5 1 calc PR . . H33A H 0.3827 0.0384 0.9734 0.108 Uiso 0.5 1 calc PR . . C34 C 0.31903(14) 0.2951(2) 0.7507(3) 0.0413(9) Uani 1 1 d . . . H34C H 0.3352 0.3505 0.7714 0.062 Uiso 1 1 calc R . . H34B H 0.2895 0.2792 0.8007 0.062 Uiso 1 1 calc R . . H34A H 0.3032 0.2998 0.6797 0.062 Uiso 1 1 calc R . . C35 C 0.26396(11) 0.31648(19) 0.2992(2) 0.0225(7) Uani 1 1 d . . . C36 C 0.25115(11) 0.2787(2) 0.2012(2) 0.0258(7) Uani 1 1 d . . . C37 C 0.19558(12) 0.2763(2) 0.1676(2) 0.0326(8) Uani 1 1 d . . . H37 H 0.1872 0.2508 0.1014 0.039 Uiso 1 1 calc R . . C38 C 0.15238(12) 0.3095(2) 0.2271(3) 0.0328(8) Uani 1 1 d . . . C39 C 0.16543(11) 0.3437(2) 0.3246(3) 0.0339(8) Uani 1 1 d . . . H39 H 0.1361 0.3659 0.3672 0.041 Uiso 1 1 calc R . . C40 C 0.22019(12) 0.3468(2) 0.3627(2) 0.0282(7) Uani 1 1 d . . . C41 C 0.29603(13) 0.2394(2) 0.1325(2) 0.0412(9) Uani 1 1 d . . . H41C H 0.3171 0.2852 0.0973 0.062 Uiso 1 1 calc R . . H41B H 0.2786 0.2022 0.0794 0.062 Uiso 1 1 calc R . . H41A H 0.3215 0.2052 0.1764 0.062 Uiso 1 1 calc R . . C42 C 0.09226(13) 0.3090(3) 0.1880(3) 0.0500(10) Uani 1 1 d . . . H42F H 0.0688 0.2773 0.2379 0.075 Uiso 0.5 1 calc PR . . H42E H 0.0906 0.2812 0.1186 0.075 Uiso 0.5 1 calc PR . . H42D H 0.0787 0.3683 0.1821 0.075 Uiso 0.5 1 calc PR . . H42C H 0.0899 0.3406 0.1212 0.075 Uiso 0.5 1 calc PR . . H42B H 0.0681 0.3366 0.2405 0.075 Uiso 0.5 1 calc PR . . H42A H 0.08 0.2496 0.177 0.075 Uiso 0.5 1 calc PR . . C43 C 0.23036(13) 0.3805(2) 0.4722(2) 0.0373(8) Uani 1 1 d . . . H43C H 0.2487 0.4368 0.468 0.056 Uiso 1 1 calc R . . H43B H 0.2545 0.3404 0.5108 0.056 Uiso 1 1 calc R . . H43A H 0.1946 0.3863 0.5093 0.056 Uiso 1 1 calc R . . C44 C 0.24275(15) 0.1372(3) 0.5140(4) 0.0628(12) Uani 1 1 d . . . H44C H 0.2264 0.161 0.4494 0.094 Uiso 1 1 calc R . . H44B H 0.2637 0.1822 0.5509 0.094 Uiso 1 1 calc R . . H44A H 0.2128 0.1157 0.5598 0.094 Uiso 1 1 calc R . . C45 C 0.31904(15) 0.0052(2) 0.6068(3) 0.0462(9) Uani 1 1 d . . . H45C H 0.3286 0.0536 0.653 0.069 Uiso 1 1 calc R . . H45B H 0.3526 -0.0292 0.5934 0.069 Uiso 1 1 calc R . . H45A H 0.2906 -0.0307 0.6411 0.069 Uiso 1 1 calc R . . C46 C 0.24927(14) -0.0422(3) 0.4209(3) 0.0572(10) Uani 1 1 d . . . H46C H 0.274 -0.0906 0.4045 0.086 Uiso 1 1 calc R . . H46B H 0.2312 -0.0221 0.3561 0.086 Uiso 1 1 calc R . . H46A H 0.2207 -0.0607 0.4714 0.086 Uiso 1 1 calc R . . C47 C 0.41146(15) -0.0746(2) 0.3811(3) 0.0444(9) Uani 1 1 d . . . H47C H 0.3811 -0.1103 0.4088 0.067 Uiso 1 1 calc R . . H47B H 0.436 -0.0569 0.4391 0.067 Uiso 1 1 calc R . . H47A H 0.4331 -0.1077 0.3294 0.067 Uiso 1 1 calc R . . C48 C 0.34162(16) -0.0173(3) 0.1981(3) 0.0526(11) Uani 1 1 d . . . H48C H 0.3256 0.0312 0.1592 0.079 Uiso 1 1 calc R . . H48B H 0.3115 -0.0554 0.2218 0.079 Uiso 1 1 calc R . . H48A H 0.3671 -0.0492 0.1519 0.079 Uiso 1 1 calc R . . C49 C 0.44031(14) 0.0898(2) 0.2620(3) 0.0416(9) Uani 1 1 d . . . H49C H 0.4629 0.1117 0.3206 0.062 Uiso 1 1 calc R . . H49B H 0.4253 0.1382 0.2214 0.062 Uiso 1 1 calc R . . H49A H 0.4637 0.054 0.216 0.062 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 Mn 0.0255(2) 0.0204(2) 0.0195(2) -0.0011(2) -0.00173(19) -0.0007(2) P1 0.0206(4) 0.0251(5) 0.0181(3) 0.0002(3) -0.0007(3) -0.0001(4) P2 0.0252(4) 0.0257(5) 0.0182(4) 0.0024(3) -0.0008(3) 0.0004(3) Si1 0.0273(4) 0.0273(5) 0.0348(4) 0.0002(4) 0.0038(4) -0.0034(4) Si2 0.0410(5) 0.0241(5) 0.0265(4) -0.0056(4) 0.0039(4) -0.0015(4) N1 0.0211(12) 0.0206(15) 0.0212(13) -0.0010(10) 0.0003(10) -0.0011(10) N2 0.0232(12) 0.0249(15) 0.0207(12) 0.0023(11) -0.0018(10) -0.0007(10) N3 0.0266(12) 0.0220(15) 0.0237(13) -0.0017(11) 0.0017(10) -0.0003(11) C1 0.0233(16) 0.035(2) 0.0220(16) 0.0025(13) 0.0025(13) -0.0001(14) C2 0.0322(17) 0.0209(19) 0.0240(15) 0.0017(13) 0.0027(13) -0.0022(14) C3 0.0301(18) 0.026(2) 0.0330(17) 0.0029(14) 0.0035(14) -0.0003(15) C4 0.0405(19) 0.035(2) 0.0441(19) 0.0035(17) 0.0088(16) 0.0099(17) C5 0.060(2) 0.033(2) 0.051(2) -0.0122(18) 0.0145(19) 0.000(2) C6 0.054(2) 0.044(3) 0.066(2) -0.030(2) 0.000(2) -0.010(2) C7 0.0345(18) 0.037(2) 0.045(2) -0.0099(17) 0.0050(15) -0.0053(16) C8 0.0212(15) 0.0227(19) 0.0291(16) -0.0014(13) -0.0048(12) -0.0010(13) C9 0.0253(16) 0.041(2) 0.0340(17) 0.0010(16) 0.0012(14) 0.0016(14) C10 0.0244(17) 0.054(3) 0.055(2) -0.0030(19) 0.0036(16) 0.0018(16) C11 0.0225(17) 0.055(3) 0.066(3) 0.009(2) -0.0129(18) 0.0009(17) C12 0.0342(19) 0.044(3) 0.046(2) 0.0125(17) -0.0188(17) -0.0068(17) C13 0.0331(18) 0.037(2) 0.0280(16) 0.0012(15) -0.0057(14) -0.0062(15) C14 0.0363(16) 0.0236(19) 0.0197(14) 0.0048(13) 0.0027(13) -0.0028(14) C15 0.0388(18) 0.028(2) 0.051(2) -0.0023(17) 0.0034(17) 0.0010(16) C16 0.052(2) 0.038(3) 0.059(2) 0.008(2) 0.011(2) 0.0091(19) C17 0.097(3) 0.028(2) 0.0352(19) 0.0052(17) 0.015(2) 0.010(2) C18 0.103(3) 0.028(2) 0.0270(17) 0.0027(18) -0.009(2) -0.017(2) C19 0.057(2) 0.028(2) 0.0304(18) 0.0085(15) -0.0078(15) -0.0096(17) C20 0.0289(16) 0.030(2) 0.0198(15) 0.0015(14) -0.0007(13) -0.0031(15) C21 0.044(2) 0.039(2) 0.0294(18) 0.0029(16) 0.0048(15) 0.0016(18) C22 0.055(2) 0.047(3) 0.038(2) -0.0045(18) 0.0140(17) 0.0016(19) C23 0.062(2) 0.063(3) 0.0226(17) 0.000(2) 0.0088(17) -0.004(2) C24 0.056(2) 0.060(3) 0.0249(18) 0.0199(17) -0.0024(16) -0.010(2) C25 0.0377(18) 0.041(2) 0.0282(17) 0.0036(15) -0.0014(14) 0.0029(16) C26 0.0216(15) 0.0255(19) 0.0195(14) -0.0017(13) -0.0040(12) -0.0054(14) C27 0.0265(16) 0.031(2) 0.0236(15) 0.0022(14) -0.0039(13) -0.0013(15) C28 0.0351(18) 0.035(2) 0.0368(18) 0.0068(16) -0.0064(15) 0.0016(16) C29 0.044(2) 0.054(3) 0.0232(17) 0.0116(16) -0.0056(15) -0.0091(18) C30 0.0428(18) 0.044(2) 0.0210(16) -0.0001(15) 0.0060(14) -0.0129(17) C31 0.0308(16) 0.028(2) 0.0220(15) -0.0058(13) 0.0054(13) -0.0063(15) C32 0.0332(18) 0.036(2) 0.0360(18) -0.0022(15) 0.0002(15) 0.0081(16) C33 0.082(3) 0.094(4) 0.040(2) 0.035(2) -0.008(2) -0.002(3) C34 0.046(2) 0.034(2) 0.0439(19) -0.0007(17) 0.0244(16) 0.0059(18) C35 0.0247(15) 0.0196(18) 0.0233(15) 0.0043(13) -0.0008(12) 0.0013(13) C36 0.0269(16) 0.023(2) 0.0279(16) 0.0007(14) -0.0021(13) 0.0007(13) C37 0.0334(18) 0.033(2) 0.0310(17) -0.0033(15) -0.0066(14) -0.0030(15) C38 0.0264(17) 0.026(2) 0.0455(19) 0.0070(16) -0.0060(14) -0.0031(15) C39 0.0262(16) 0.036(2) 0.0395(19) 0.0047(17) 0.0054(15) 0.0046(14) C40 0.0294(17) 0.027(2) 0.0283(16) 0.0025(14) 0.0027(13) 0.0017(14) C41 0.0386(19) 0.050(3) 0.0350(18) -0.0179(17) -0.0046(15) 0.0005(18) C42 0.0319(18) 0.056(3) 0.062(2) 0.004(2) -0.0125(17) 0.0014(18) C43 0.0335(17) 0.046(2) 0.0326(17) -0.0096(17) 0.0055(15) 0.0026(16) C44 0.048(2) 0.051(3) 0.089(3) 0.021(2) 0.035(2) 0.0144(19) C45 0.051(2) 0.045(3) 0.043(2) 0.0071(18) 0.0025(17) -0.0093(19) C46 0.053(2) 0.064(3) 0.054(2) 0.001(2) 0.001(2) -0.0281(19) C47 0.055(2) 0.030(2) 0.048(2) -0.0023(17) 0.0111(16) 0.0086(18) C48 0.070(3) 0.055(3) 0.0323(19) -0.0144(18) 0.0039(18) -0.009(2) C49 0.046(2) 0.039(2) 0.0406(19) -0.0029(17) 0.0137(16) 0.0014(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn N3 2.012(2) . ? Mn N1 2.110(2) . ? Mn N2 2.124(2) . ? P1 N1 1.618(2) . ? P1 C1 1.735(3) . ? P1 C8 1.811(3) . ? P1 C2 1.822(3) . ? P2 N2 1.609(2) . ? P2 C1 1.717(3) . ? P2 C14 1.818(3) . ? P2 C20 1.831(3) . ? Si1 N3 1.712(2) . ? Si1 C46 1.862(4) . ? Si1 C45 1.865(3) . ? Si1 C44 1.870(4) . ? Si2 N3 1.700(2) . ? Si2 C48 1.873(3) . ? Si2 C49 1.874(3) . ? Si2 C47 1.888(4) . ? N1 C26 1.442(3) . ? N2 C35 1.437(3) . ? C2 C7 1.392(4) . ? C2 C3 1.396(4) . ? C3 C4 1.383(5) . ? C4 C5 1.360(5) . ? C5 C6 1.386(5) . ? C6 C7 1.378(5) . ? C8 C9 1.391(4) . ? C8 C13 1.398(4) . ? C9 C10 1.381(4) . ? C10 C11 1.377(5) . ? C11 C12 1.365(5) . ? C12 C13 1.393(4) . ? C14 C19 1.393(4) . ? C14 C15 1.398(4) . ? C15 C16 1.370(5) . ? C16 C17 1.373(5) . ? C17 C18 1.365(5) . ? C18 C19 1.392(5) . ? C20 C25 1.386(4) . ? C20 C21 1.396(4) . ? C21 C22 1.383(4) . ? C22 C23 1.380(5) . ? C23 C24 1.370(5) . ? C24 C25 1.397(4) . ? C26 C31 1.404(4) . ? C26 C27 1.405(4) . ? C27 C28 1.389(4) . ? C27 C32 1.509(4) . ? C28 C29 1.372(5) . ? C29 C30 1.382(5) . ? C29 C33 1.521(4) . ? C30 C31 1.393(4) . ? C31 C34 1.499(4) . ? C35 C40 1.402(4) . ? C35 C36 1.408(4) . ? C36 C37 1.395(4) . ? C36 C41 1.511(4) . ? C37 C38 1.379(4) . ? C38 C39 1.381(4) . ? C38 C42 1.520(4) . ? C39 C40 1.396(4) . ? C40 C43 1.504(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 N3 Mn N1 120.27(9) . . ? N3 Mn N2 126.76(9) . . ? N1 Mn N2 109.16(9) . . ? N1 P1 C1 107.10(14) . . ? N1 P1 C8 112.13(13) . . ? C1 P1 C8 108.07(13) . . ? N1 P1 C2 112.02(12) . . ? C1 P1 C2 113.92(15) . . ? C8 P1 C2 103.62(13) . . ? N2 P2 C1 106.12(14) . . ? N2 P2 C14 113.33(13) . . ? C1 P2 C14 114.58(15) . . ? N2 P2 C20 115.60(13) . . ? C1 P2 C20 104.75(14) . . ? C14 P2 C20 102.42(14) . . ? N3 Si1 C46 113.83(15) . . ? N3 Si1 C45 113.12(14) . . ? C46 Si1 C45 106.12(18) . . ? N3 Si1 C44 108.43(15) . . ? C46 Si1 C44 108.75(19) . . ? C45 Si1 C44 106.26(18) . . ? N3 Si2 C48 113.79(15) . . ? N3 Si2 C49 108.91(14) . . ? C48 Si2 C49 106.32(17) . . ? N3 Si2 C47 113.69(13) . . ? C48 Si2 C47 105.48(18) . . ? C49 Si2 C47 108.27(16) . . ? C26 N1 P1 122.86(18) . . ? C26 N1 Mn 128.33(18) . . ? P1 N1 Mn 104.62(11) . . ? C35 N2 P2 130.02(19) . . ? C35 N2 Mn 124.57(18) . . ? P2 N2 Mn 104.99(11) . . ? Si2 N3 Si1 124.14(15) . . ? Si2 N3 Mn 122.24(13) . . ? Si1 N3 Mn 113.26(12) . . ? P2 C1 P1 130.73(18) . . ? C7 C2 C3 118.1(3) . . ? C7 C2 P1 123.7(2) . . ? C3 C2 P1 118.2(2) . . ? C4 C3 C2 121.0(3) . . ? C5 C4 C3 120.3(3) . . ? C4 C5 C6 119.4(3) . . ? C7 C6 C5 121.0(3) . . ? C6 C7 C2 120.0(3) . . ? C9 C8 C13 118.2(3) . . ? C9 C8 P1 123.9(2) . . ? C13 C8 P1 117.6(2) . . ? C10 C9 C8 120.6(3) . . ? C11 C10 C9 120.8(3) . . ? C12 C11 C10 119.5(3) . . ? C11 C12 C13 120.8(3) . . ? C12 C13 C8 120.1(3) . . ? C19 C14 C15 118.0(3) . . ? C19 C14 P2 120.2(2) . . ? C15 C14 P2 121.7(2) . . ? C16 C15 C14 121.5(3) . . ? C15 C16 C17 119.6(4) . . ? C18 C17 C16 120.4(4) . . ? C17 C18 C19 120.7(3) . . ? C18 C19 C14 119.8(3) . . ? C25 C20 C21 118.3(3) . . ? C25 C20 P2 122.3(2) . . ? C21 C20 P2 119.3(2) . . ? C22 C21 C20 120.9(3) . . ? C23 C22 C21 120.2(3) . . ? C24 C23 C22 119.6(3) . . ? C23 C24 C25 120.7(3) . . ? C20 C25 C24 120.2(3) . . ? C31 C26 C27 118.8(3) . . ? C31 C26 N1 121.8(3) . . ? C27 C26 N1 119.3(2) . . ? C28 C27 C26 119.4(3) . . ? C28 C27 C32 118.3(3) . . ? C26 C27 C32 122.4(3) . . ? C29 C28 C27 122.7(3) . . ? C28 C29 C30 117.4(3) . . ? C28 C29 C33 122.0(3) . . ? C30 C29 C33 120.5(3) . . ? C29 C30 C31 122.5(3) . . ? C30 C31 C26 119.1(3) . . ? C30 C31 C34 118.2(3) . . ? C26 C31 C34 122.7(3) . . ? C40 C35 C36 119.0(2) . . ? C40 C35 N2 119.9(2) . . ? C36 C35 N2 120.8(2) . . ? C37 C36 C35 119.1(3) . . ? C37 C36 C41 119.3(3) . . ? C35 C36 C41 121.5(2) . . ? C38 C37 C36 122.4(3) . . ? C37 C38 C39 117.7(3) . . ? C37 C38 C42 121.9(3) . . ? C39 C38 C42 120.5(3) . . ? C38 C39 C40 122.3(3) . . ? C39 C40 C35 119.3(3) . . ? C39 C40 C43 118.9(3) . . ? C35 C40 C43 121.8(3) . . ? #===END data_apr202 _database_code_CSD 191081 _audit_creation_date 2002-04-08T11:40:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Fe{N(SiMe3)2}{MesNPPh2CHPPh2NMes}] _chemical_formula_moiety 'C49 H61 Fe N3 P2 Si2' _chemical_formula_sum 'C49 H61 Fe N3 P2 Si2' _chemical_formula_weight 865.98 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 11.9774(3) _cell_length_b 18.4685(4) _cell_length_c 21.5940(7) _cell_angle_alpha 90 _cell_angle_beta 94.420(1) _cell_angle_gamma 90 _cell_volume 4762.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13569 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.47 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.971 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.82311E-1 _diffrn_orient_matrix_UB_12 0.98156E-2 _diffrn_orient_matrix_UB_13 0.20774E-2 _diffrn_orient_matrix_UB_21 0.107199E-1 _diffrn_orient_matrix_UB_22 -0.299292E-1 _diffrn_orient_matrix_UB_23 0.385919E-1 _diffrn_orient_matrix_UB_31 0.110597E-1 _diffrn_orient_matrix_UB_32 -0.440422E-1 _diffrn_orient_matrix_UB_33 -0.257624E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_number 24917 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 23.04 _diffrn_reflns_theta_full 23.04 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 6580 _reflns_number_gt 5041 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+5.2924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 6580 _refine_ls_number_parameters 528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.242 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.69167(4) 0.23796(3) 0.10559(2) 0.02951(15) Uani 1 1 d . . . P1 P 0.93947(7) 0.24142(5) 0.15823(4) 0.0284(2) Uani 1 1 d . . . P2 P 0.87670(7) 0.24026(5) 0.01294(4) 0.0292(2) Uani 1 1 d . . . Si1 Si 0.44860(9) 0.27567(6) 0.13457(5) 0.0451(3) Uani 1 1 d . . . Si2 Si 0.50401(10) 0.11830(6) 0.11515(6) 0.0510(3) Uani 1 1 d . . . N1 N 0.8106(2) 0.25913(15) 0.17277(12) 0.0315(7) Uani 1 1 d . . . N2 N 0.7518(2) 0.26715(15) 0.02557(13) 0.0315(7) Uani 1 1 d . . . N3 N 0.5405(2) 0.20806(16) 0.11817(14) 0.0351(7) Uani 1 1 d . . . C1 C 0.9486(3) 0.2193(2) 0.08190(16) 0.0324(8) Uani 1 1 d . . . H1 H 0.998(3) 0.187(2) 0.0784(18) 0.049(12) Uiso 1 1 d . . . C2 C 1.0280(3) 0.31538(18) 0.18819(16) 0.0315(8) Uani 1 1 d . . . C3 C 1.0757(3) 0.36205(19) 0.14702(18) 0.0401(9) Uani 1 1 d . . . H3 H 1.0648 0.3538 0.1035 0.048 Uiso 1 1 calc R . . C4 C 1.1393(3) 0.4208(2) 0.1695(2) 0.0504(11) Uani 1 1 d . . . H4 H 1.1711 0.4527 0.1413 0.06 Uiso 1 1 calc R . . C5 C 1.1565(3) 0.4329(2) 0.2322(2) 0.0500(11) Uani 1 1 d . . . H5 H 1.2013 0.4725 0.2472 0.06 Uiso 1 1 calc R . . C6 C 1.1087(3) 0.3875(2) 0.27340(19) 0.0457(10) Uani 1 1 d . . . H6 H 1.1196 0.3965 0.3168 0.055 Uiso 1 1 calc R . . C7 C 1.0448(3) 0.32871(19) 0.25196(17) 0.0375(9) Uani 1 1 d . . . H7 H 1.0125 0.2975 0.2806 0.045 Uiso 1 1 calc R . . C8 C 0.9991(3) 0.16189(19) 0.19973(15) 0.0310(8) Uani 1 1 d . . . C9 C 0.9421(3) 0.09662(19) 0.19086(17) 0.0385(9) Uani 1 1 d . . . H9 H 0.8758 0.095 0.1638 0.046 Uiso 1 1 calc R . . C10 C 0.9797(3) 0.0344(2) 0.22049(18) 0.0429(10) Uani 1 1 d . . . H10 H 0.9394 -0.0096 0.2139 0.052 Uiso 1 1 calc R . . C11 C 1.0758(4) 0.0360(2) 0.25971(19) 0.0483(11) Uani 1 1 d . . . H11 H 1.1007 -0.0064 0.2814 0.058 Uiso 1 1 calc R . . C12 C 1.1352(3) 0.0990(2) 0.26731(19) 0.0489(11) Uani 1 1 d . . . H12 H 1.2029 0.0996 0.2933 0.059 Uiso 1 1 calc R . . C13 C 1.0980(3) 0.1622(2) 0.23759(18) 0.0415(9) Uani 1 1 d . . . H13 H 1.1403 0.2056 0.2432 0.05 Uiso 1 1 calc R . . C14 C 0.9469(3) 0.30551(19) -0.03450(16) 0.0339(9) Uani 1 1 d . . . C15 C 0.8941(3) 0.3392(2) -0.08709(18) 0.0426(10) Uani 1 1 d . . . H15 H 0.8191 0.3271 -0.1006 0.051 Uiso 1 1 calc R . . C16 C 0.9519(4) 0.3906(2) -0.1195(2) 0.0517(11) Uani 1 1 d . . . H16 H 0.9161 0.4135 -0.1551 0.062 Uiso 1 1 calc R . . C17 C 1.0606(4) 0.4083(2) -0.1001(2) 0.0561(12) Uani 1 1 d . . . H17 H 1.0988 0.4446 -0.1213 0.067 Uiso 1 1 calc R . . C18 C 1.1136(4) 0.3736(2) -0.0502(2) 0.0558(12) Uani 1 1 d . . . H18 H 1.1893 0.3851 -0.0378 0.067 Uiso 1 1 calc R . . C19 C 1.0586(3) 0.3223(2) -0.01793(18) 0.0418(10) Uani 1 1 d . . . H19 H 1.0973 0.298 0.0161 0.05 Uiso 1 1 calc R . . C20 C 0.8790(3) 0.15766(19) -0.03362(16) 0.0318(8) Uani 1 1 d . . . C21 C 0.8847(3) 0.1583(2) -0.09753(17) 0.0429(10) Uani 1 1 d . . . H21 H 0.8942 0.203 -0.1183 0.051 Uiso 1 1 calc R . . C22 C 0.8766(4) 0.0944(2) -0.13143(18) 0.0501(11) Uani 1 1 d . . . H22 H 0.8803 0.0956 -0.1752 0.06 Uiso 1 1 calc R . . C23 C 0.8633(4) 0.0291(2) -0.1018(2) 0.0503(11) Uani 1 1 d . . . H23 H 0.8577 -0.0146 -0.125 0.06 Uiso 1 1 calc R . . C24 C 0.8581(4) 0.0277(2) -0.03831(19) 0.0494(11) Uani 1 1 d . . . H24 H 0.8493 -0.0171 -0.0177 0.059 Uiso 1 1 calc R . . C25 C 0.8656(3) 0.0913(2) -0.00447(18) 0.0430(10) Uani 1 1 d . . . H25 H 0.8617 0.0897 0.0393 0.052 Uiso 1 1 calc R . . C26 C 0.7817(3) 0.2894(2) 0.23114(16) 0.0345(9) Uani 1 1 d . . . C27 C 0.7845(3) 0.3646(2) 0.24205(17) 0.0378(9) Uani 1 1 d . . . C28 C 0.7563(3) 0.3908(2) 0.29909(19) 0.0474(10) Uani 1 1 d . . . H28 H 0.761 0.4414 0.3067 0.057 Uiso 1 1 calc R . . C29 C 0.7215(3) 0.3461(3) 0.34518(18) 0.0502(11) Uani 1 1 d . . . C30 C 0.7134(3) 0.2729(3) 0.33245(18) 0.0487(11) Uani 1 1 d . . . H30 H 0.6872 0.2416 0.3631 0.058 Uiso 1 1 calc R . . C31 C 0.7420(3) 0.2429(2) 0.27644(17) 0.0410(9) Uani 1 1 d . . . C32 C 0.8142(4) 0.4188(2) 0.19418(19) 0.0513(11) Uani 1 1 d . . . H32C H 0.887 0.4406 0.2069 0.077 Uiso 1 1 calc R . . H32B H 0.7569 0.4567 0.1903 0.077 Uiso 1 1 calc R . . H32A H 0.8182 0.3945 0.1541 0.077 Uiso 1 1 calc R . . C33 C 0.6925(4) 0.3770(3) 0.4070(2) 0.0728(15) Uani 1 1 d . . . H33A H 0.7036 0.4295 0.4071 0.109 Uiso 0.5 1 calc PR . . H33B H 0.741 0.3552 0.4406 0.109 Uiso 0.5 1 calc PR . . H33C H 0.6141 0.3662 0.4134 0.109 Uiso 0.5 1 calc PR . . H33D H 0.6689 0.3377 0.4336 0.109 Uiso 0.5 1 calc PR . . H33E H 0.6314 0.4121 0.4001 0.109 Uiso 0.5 1 calc PR . . H33F H 0.7584 0.4011 0.4273 0.109 Uiso 0.5 1 calc PR . . C34 C 0.7255(4) 0.1645(2) 0.2650(2) 0.0629(13) Uani 1 1 d . . . H34C H 0.7984 0.1402 0.2668 0.094 Uiso 1 1 calc R . . H34B H 0.6865 0.1572 0.2239 0.094 Uiso 1 1 calc R . . H34A H 0.6806 0.1441 0.2969 0.094 Uiso 1 1 calc R . . C35 C 0.6757(3) 0.30884(19) -0.01503(15) 0.0313(8) Uani 1 1 d . . . C36 C 0.6778(3) 0.3850(2) -0.01335(16) 0.0376(9) Uani 1 1 d . . . C37 C 0.5931(3) 0.4234(2) -0.04627(18) 0.0461(10) Uani 1 1 d . . . H37 H 0.5946 0.4748 -0.0448 0.055 Uiso 1 1 calc R . . C38 C 0.5069(3) 0.3897(2) -0.08104(18) 0.0476(11) Uani 1 1 d . . . C39 C 0.5085(3) 0.3153(2) -0.08406(17) 0.0448(10) Uani 1 1 d . . . H39 H 0.4511 0.2914 -0.109 0.054 Uiso 1 1 calc R . . C40 C 0.5909(3) 0.2737(2) -0.05202(16) 0.0363(9) Uani 1 1 d . . . C41 C 0.7699(4) 0.4260(2) 0.0243(2) 0.0534(11) Uani 1 1 d . . . H41C H 0.7363 0.4591 0.0531 0.08 Uiso 1 1 calc R . . H41B H 0.814 0.4538 -0.0038 0.08 Uiso 1 1 calc R . . H41A H 0.8188 0.3916 0.0479 0.08 Uiso 1 1 calc R . . C42 C 0.4125(4) 0.4332(3) -0.1131(2) 0.0690(14) Uani 1 1 d . . . H42A H 0.3592 0.4004 -0.1355 0.104 Uiso 0.5 1 calc PR . . H42B H 0.4428 0.467 -0.1425 0.104 Uiso 0.5 1 calc PR . . H42C H 0.3741 0.4604 -0.0821 0.104 Uiso 0.5 1 calc PR . . H42D H 0.4249 0.4848 -0.1046 0.104 Uiso 0.5 1 calc PR . . H42E H 0.3413 0.4182 -0.0976 0.104 Uiso 0.5 1 calc PR . . H42F H 0.41 0.4247 -0.158 0.104 Uiso 0.5 1 calc PR . . C43 C 0.5863(4) 0.1927(2) -0.0563(2) 0.0504(11) Uani 1 1 d . . . H43C H 0.6524 0.1749 -0.0756 0.076 Uiso 1 1 calc R . . H43B H 0.5185 0.1781 -0.0815 0.076 Uiso 1 1 calc R . . H43A H 0.5849 0.1721 -0.0145 0.076 Uiso 1 1 calc R . . C44 C 0.5118(6) 0.3658(3) 0.1268(4) 0.135(3) Uani 1 1 d . . . H44C H 0.5514 0.3674 0.0888 0.202 Uiso 1 1 calc R . . H44B H 0.5648 0.3751 0.1628 0.202 Uiso 1 1 calc R . . H44A H 0.4529 0.4027 0.1247 0.202 Uiso 1 1 calc R . . C45 C 0.3224(7) 0.2756(5) 0.0803(4) 0.204(6) Uani 1 1 d . . . H45C H 0.2678 0.2412 0.0947 0.306 Uiso 1 1 calc R . . H45B H 0.3425 0.2614 0.0389 0.306 Uiso 1 1 calc R . . H45A H 0.2896 0.3243 0.0784 0.306 Uiso 1 1 calc R . . C46 C 0.4078(7) 0.2730(4) 0.2150(3) 0.131(3) Uani 1 1 d . . . H46C H 0.4749 0.2683 0.2436 0.197 Uiso 1 1 calc R . . H46B H 0.3583 0.2315 0.22 0.197 Uiso 1 1 calc R . . H46A H 0.3684 0.3178 0.224 0.197 Uiso 1 1 calc R . . C47 C 0.3953(5) 0.0961(3) 0.0517(3) 0.110(2) Uani 1 1 d . . . H47C H 0.4166 0.1171 0.0126 0.165 Uiso 1 1 calc R . . H47B H 0.3231 0.1162 0.0617 0.165 Uiso 1 1 calc R . . H47A H 0.3889 0.0435 0.0474 0.165 Uiso 1 1 calc R . . C48 C 0.4479(6) 0.0852(3) 0.1882(3) 0.113(3) Uani 1 1 d . . . H48C H 0.3728 0.105 0.1916 0.169 Uiso 1 1 calc R . . H48B H 0.4974 0.1009 0.2239 0.169 Uiso 1 1 calc R . . H48A H 0.4441 0.0322 0.1875 0.169 Uiso 1 1 calc R . . C49 C 0.6265(4) 0.0607(2) 0.1011(3) 0.0665(13) Uani 1 1 d . . . H49C H 0.686 0.0688 0.1341 0.1 Uiso 1 1 calc R . . H49B H 0.654 0.0732 0.0609 0.1 Uiso 1 1 calc R . . H49A H 0.6042 0.0096 0.1009 0.1 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 Fe 0.0231(3) 0.0348(3) 0.0310(3) 0.0024(2) 0.0045(2) 0.0002(2) P1 0.0251(5) 0.0335(5) 0.0266(5) 0.0004(4) 0.0025(4) 0.0017(4) P2 0.0259(5) 0.0352(5) 0.0269(5) 0.0009(4) 0.0037(4) 0.0005(4) Si1 0.0292(6) 0.0612(8) 0.0458(7) -0.0013(5) 0.0080(5) 0.0077(5) Si2 0.0393(7) 0.0490(7) 0.0659(8) 0.0050(6) 0.0120(6) -0.0123(5) N1 0.0274(16) 0.0412(17) 0.0262(16) -0.0011(13) 0.0044(12) 0.0014(13) N2 0.0290(16) 0.0365(17) 0.0294(16) 0.0028(13) 0.0046(13) 0.0044(13) N3 0.0247(16) 0.0414(18) 0.0397(18) 0.0036(14) 0.0059(13) -0.0015(13) C1 0.030(2) 0.037(2) 0.030(2) -0.0026(16) 0.0029(16) 0.0095(17) C2 0.0243(19) 0.034(2) 0.036(2) -0.0038(16) 0.0040(16) 0.0018(15) C3 0.043(2) 0.037(2) 0.042(2) 0.0005(17) 0.0119(18) 0.0026(17) C4 0.048(3) 0.038(2) 0.067(3) 0.000(2) 0.021(2) -0.0074(19) C5 0.041(2) 0.042(2) 0.067(3) -0.017(2) 0.011(2) -0.0085(19) C6 0.041(2) 0.053(3) 0.042(2) -0.012(2) -0.0018(19) -0.0026(19) C7 0.035(2) 0.038(2) 0.039(2) -0.0018(17) 0.0027(17) 0.0005(17) C8 0.028(2) 0.041(2) 0.0251(19) 0.0006(15) 0.0050(16) 0.0058(16) C9 0.034(2) 0.040(2) 0.041(2) -0.0004(18) 0.0002(17) -0.0004(17) C10 0.042(2) 0.038(2) 0.050(2) 0.0030(19) 0.013(2) 0.0040(18) C11 0.048(3) 0.048(3) 0.050(3) 0.012(2) 0.011(2) 0.020(2) C12 0.040(2) 0.060(3) 0.045(3) 0.006(2) -0.007(2) 0.014(2) C13 0.036(2) 0.043(2) 0.044(2) -0.0019(18) -0.0041(19) 0.0053(17) C14 0.034(2) 0.039(2) 0.030(2) -0.0013(16) 0.0100(17) 0.0005(16) C15 0.041(2) 0.049(2) 0.039(2) 0.0081(19) 0.0106(19) 0.0054(18) C16 0.065(3) 0.045(3) 0.047(3) 0.015(2) 0.019(2) 0.011(2) C17 0.071(3) 0.048(3) 0.053(3) 0.001(2) 0.032(3) -0.016(2) C18 0.055(3) 0.067(3) 0.048(3) -0.008(2) 0.020(2) -0.021(2) C19 0.035(2) 0.057(3) 0.034(2) -0.0029(18) 0.0126(18) -0.0069(18) C20 0.0259(19) 0.040(2) 0.030(2) -0.0029(16) 0.0058(16) 0.0021(15) C21 0.051(3) 0.048(2) 0.030(2) -0.0020(18) 0.0053(18) 0.0065(18) C22 0.060(3) 0.061(3) 0.029(2) -0.011(2) 0.007(2) 0.003(2) C23 0.052(3) 0.050(3) 0.050(3) -0.019(2) 0.008(2) -0.004(2) C24 0.059(3) 0.045(3) 0.046(3) -0.003(2) 0.011(2) -0.009(2) C25 0.052(3) 0.044(2) 0.034(2) -0.0059(18) 0.0109(19) -0.0049(19) C26 0.024(2) 0.052(2) 0.027(2) -0.0005(17) 0.0022(15) 0.0057(16) C27 0.028(2) 0.049(2) 0.036(2) -0.0044(18) 0.0055(17) 0.0070(17) C28 0.035(2) 0.058(3) 0.049(3) -0.017(2) 0.003(2) 0.0044(19) C29 0.031(2) 0.086(3) 0.034(2) -0.014(2) 0.0053(18) 0.001(2) C30 0.036(2) 0.077(3) 0.034(2) 0.004(2) 0.0074(18) 0.001(2) C31 0.033(2) 0.057(3) 0.033(2) 0.0084(18) 0.0056(17) 0.0067(18) C32 0.056(3) 0.048(3) 0.051(3) 0.001(2) 0.013(2) 0.012(2) C33 0.059(3) 0.118(4) 0.043(3) -0.029(3) 0.016(2) -0.015(3) C34 0.085(4) 0.055(3) 0.054(3) 0.014(2) 0.035(3) 0.003(2) C35 0.027(2) 0.044(2) 0.0238(19) 0.0039(16) 0.0052(15) 0.0033(16) C36 0.042(2) 0.042(2) 0.030(2) 0.0009(17) 0.0088(17) 0.0067(17) C37 0.047(3) 0.051(2) 0.042(2) 0.0093(19) 0.013(2) 0.015(2) C38 0.037(2) 0.070(3) 0.037(2) 0.020(2) 0.009(2) 0.014(2) C39 0.031(2) 0.070(3) 0.033(2) 0.0041(19) 0.0000(18) 0.0009(19) C40 0.028(2) 0.051(2) 0.030(2) 0.0010(17) 0.0023(16) -0.0016(17) C41 0.067(3) 0.041(2) 0.051(3) -0.0053(19) -0.004(2) 0.000(2) C42 0.044(3) 0.100(4) 0.063(3) 0.034(3) 0.005(2) 0.022(3) C43 0.043(3) 0.055(3) 0.051(3) -0.010(2) -0.006(2) -0.0097(19) C44 0.113(6) 0.054(4) 0.250(9) 0.013(4) 0.096(6) 0.029(3) C45 0.128(7) 0.268(11) 0.199(9) -0.151(8) -0.107(6) 0.145(7) C46 0.192(8) 0.117(5) 0.096(5) 0.023(4) 0.092(5) 0.072(5) C47 0.073(4) 0.104(5) 0.149(6) -0.015(4) -0.025(4) -0.041(3) C48 0.144(6) 0.070(4) 0.136(6) 0.019(4) 0.086(5) -0.023(4) C49 0.061(3) 0.041(3) 0.098(4) -0.004(2) 0.009(3) -0.005(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N3 1.932(3) . ? Fe N1 1.992(3) . ? Fe N2 1.997(3) . ? P1 N1 1.632(3) . ? P1 C1 1.710(4) . ? P1 C2 1.817(4) . ? P1 C8 1.836(3) . ? P2 N2 1.620(3) . ? P2 C1 1.706(4) . ? P2 C14 1.828(4) . ? P2 C20 1.828(3) . ? Si1 N3 1.719(3) . ? Si1 C44 1.841(6) . ? Si1 C46 1.840(5) . ? Si1 C45 1.840(6) . ? Si2 N3 1.714(3) . ? Si2 C49 1.856(5) . ? Si2 C47 1.861(6) . ? Si2 C48 1.865(5) . ? N1 C26 1.445(4) . ? N2 C35 1.438(4) . ? C2 C3 1.392(5) . ? C2 C7 1.398(5) . ? C3 C4 1.391(5) . ? C4 C5 1.371(6) . ? C5 C6 1.379(6) . ? C6 C7 1.387(5) . ? C8 C13 1.387(5) . ? C8 C9 1.391(5) . ? C9 C10 1.374(5) . ? C10 C11 1.376(6) . ? C11 C12 1.368(6) . ? C12 C13 1.388(5) . ? C14 C19 1.393(5) . ? C14 C15 1.402(5) . ? C15 C16 1.395(5) . ? C16 C17 1.377(6) . ? C17 C18 1.365(6) . ? C18 C19 1.374(5) . ? C20 C21 1.387(5) . ? C20 C25 1.393(5) . ? C21 C22 1.389(5) . ? C22 C23 1.380(6) . ? C23 C24 1.377(6) . ? C24 C25 1.383(5) . ? C26 C27 1.408(5) . ? C26 C31 1.412(5) . ? C27 C28 1.389(5) . ? C27 C32 1.502(5) . ? C28 C29 1.382(6) . ? C29 C30 1.381(6) . ? C29 C33 1.517(6) . ? C30 C31 1.396(5) . ? C31 C34 1.481(6) . ? C35 C40 1.402(5) . ? C35 C36 1.407(5) . ? C36 C37 1.388(5) . ? C36 C41 1.521(5) . ? C37 C38 1.377(6) . ? C38 C39 1.376(6) . ? C38 C42 1.511(5) . ? C39 C40 1.392(5) . ? C40 C43 1.500(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 N3 Fe N1 125.37(12) . . ? N3 Fe N2 127.09(12) . . ? N1 Fe N2 106.99(11) . . ? N1 P1 C1 111.40(16) . . ? N1 P1 C2 108.38(15) . . ? C1 P1 C2 116.37(17) . . ? N1 P1 C8 113.85(15) . . ? C1 P1 C8 103.17(17) . . ? C2 P1 C8 103.50(16) . . ? N2 P2 C1 109.46(16) . . ? N2 P2 C14 111.30(15) . . ? C1 P2 C14 114.57(18) . . ? N2 P2 C20 113.67(15) . . ? C1 P2 C20 105.22(17) . . ? C14 P2 C20 102.41(16) . . ? N3 Si1 C44 111.3(2) . . ? N3 Si1 C46 113.3(2) . . ? C44 Si1 C46 104.5(4) . . ? N3 Si1 C45 112.1(2) . . ? C44 Si1 C45 105.4(5) . . ? C46 Si1 C45 109.6(5) . . ? N3 Si2 C49 110.99(18) . . ? N3 Si2 C47 113.7(2) . . ? C49 Si2 C47 105.7(3) . . ? N3 Si2 C48 113.1(2) . . ? C49 Si2 C48 106.9(3) . . ? C47 Si2 C48 105.8(3) . . ? C26 N1 P1 122.6(2) . . ? C26 N1 Fe 120.4(2) . . ? P1 N1 Fe 117.02(15) . . ? C35 N2 P2 127.7(2) . . ? C35 N2 Fe 114.7(2) . . ? P2 N2 Fe 117.54(15) . . ? Si2 N3 Si1 123.02(18) . . ? Si2 N3 Fe 120.66(16) . . ? Si1 N3 Fe 116.30(16) . . ? P2 C1 P1 136.2(2) . . ? C3 C2 C7 119.0(3) . . ? C3 C2 P1 119.7(3) . . ? C7 C2 P1 121.3(3) . . ? C4 C3 C2 120.0(4) . . ? C5 C4 C3 120.6(4) . . ? C4 C5 C6 119.9(4) . . ? C5 C6 C7 120.4(4) . . ? C6 C7 C2 120.0(4) . . ? C13 C8 C9 118.2(3) . . ? C13 C8 P1 124.5(3) . . ? C9 C8 P1 117.2(3) . . ? C10 C9 C8 121.4(4) . . ? C9 C10 C11 119.8(4) . . ? C12 C11 C10 119.7(4) . . ? C11 C12 C13 120.9(4) . . ? C8 C13 C12 119.9(4) . . ? C19 C14 C15 118.2(3) . . ? C19 C14 P2 118.5(3) . . ? C15 C14 P2 123.2(3) . . ? C16 C15 C14 119.9(4) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 120.1(4) . . ? C17 C18 C19 120.7(4) . . ? C18 C19 C14 120.8(4) . . ? C21 C20 C25 118.3(3) . . ? C21 C20 P2 122.9(3) . . ? C25 C20 P2 118.6(3) . . ? C20 C21 C22 120.7(4) . . ? C23 C22 C21 120.3(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 120.3(4) . . ? C24 C25 C20 120.9(4) . . ? C27 C26 C31 119.2(3) . . ? C27 C26 N1 121.6(3) . . ? C31 C26 N1 119.0(3) . . ? C28 C27 C26 119.2(4) . . ? C28 C27 C32 117.7(4) . . ? C26 C27 C32 123.1(3) . . ? C29 C28 C27 122.5(4) . . ? C30 C29 C28 117.5(4) . . ? C30 C29 C33 121.7(4) . . ? C28 C29 C33 120.7(4) . . ? C29 C30 C31 122.8(4) . . ? C30 C31 C26 118.5(4) . . ? C30 C31 C34 119.6(4) . . ? C26 C31 C34 121.9(3) . . ? C40 C35 C36 119.2(3) . . ? C40 C35 N2 119.8(3) . . ? C36 C35 N2 120.7(3) . . ? C37 C36 C35 119.1(4) . . ? C37 C36 C41 119.4(3) . . ? C35 C36 C41 121.5(3) . . ? C38 C37 C36 122.5(4) . . ? C37 C38 C39 117.6(4) . . ? C37 C38 C42 120.9(4) . . ? C39 C38 C42 121.4(4) . . ? C38 C39 C40 122.7(4) . . ? C39 C40 C35 118.8(4) . . ? C39 C40 C43 119.9(4) . . ? C35 C40 C43 121.2(3) . . ? #===END data_apr1102 _database_code_CSD 198769 _audit_creation_date 2002-04-19T17:44:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Co{N(SiMe3)2}(MesNPPh2CHPPh2NMes)] _chemical_formula_moiety 'C49 H61 Co1 N3 P2 Si2' _chemical_formula_sum 'C49 H61 Co N3 P2 Si2' _chemical_formula_weight 869.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2503(6) _cell_length_b 19.5120(9) _cell_length_c 19.5346(10) _cell_angle_alpha 90 _cell_angle_beta 94.046(2) _cell_angle_gamma 90 _cell_volume 4657.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29875 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.941 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_av_unetI/netI 0.0795 _diffrn_reflns_number 20510 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 6409 _reflns_number_gt 4662 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+3.5314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 6409 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.361 _refine_diff_density_min -0.55 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.74029(4) 0.76453(3) 0.04940(2) 0.02710(17) Uani 1 1 d . . . P1 P 0.77168(8) 0.76215(5) 0.19339(5) 0.0271(3) Uani 1 1 d . . . P2 P 0.89226(8) 0.66159(5) 0.09493(5) 0.0277(3) Uani 1 1 d . . . Si1 Si 0.61922(10) 0.82004(6) -0.07644(6) 0.0381(3) Uani 1 1 d . . . Si2 Si 0.82278(10) 0.89878(6) -0.03340(6) 0.0384(3) Uani 1 1 d . . . N1 N 0.6688(3) 0.77213(15) 0.13779(15) 0.0278(8) Uani 1 1 d . . . N2 N 0.7941(3) 0.66929(15) 0.03549(16) 0.0298(8) Uani 1 1 d . . . N3 N 0.7348(3) 0.83221(15) -0.02309(16) 0.0313(8) Uani 1 1 d . . . C1 C 0.8785(3) 0.73115(19) 0.14895(19) 0.0297(9) Uani 1 1 d . . . H1 H 0.9432 0.7578 0.1555 0.036 Uiso 1 1 calc R . . C2 C 0.7345(3) 0.7148(2) 0.26798(19) 0.0289(9) Uani 1 1 d . . . C3 C 0.7768(3) 0.6503(2) 0.2826(2) 0.0378(11) Uani 1 1 d . . . H3 H 0.826 0.6304 0.2528 0.045 Uiso 1 1 calc R . . C4 C 0.7492(4) 0.6144(2) 0.3396(2) 0.0448(12) Uani 1 1 d . . . H4 H 0.7799 0.5704 0.3491 0.054 Uiso 1 1 calc R . . C5 C 0.6775(4) 0.6421(2) 0.3825(2) 0.0472(12) Uani 1 1 d . . . H5 H 0.6577 0.617 0.4214 0.057 Uiso 1 1 calc R . . C6 C 0.6342(4) 0.7059(2) 0.3696(2) 0.0475(12) Uani 1 1 d . . . H6 H 0.5853 0.7252 0.4 0.057 Uiso 1 1 calc R . . C7 C 0.6613(4) 0.7425(2) 0.3126(2) 0.0392(11) Uani 1 1 d . . . H7 H 0.6303 0.7865 0.3036 0.047 Uiso 1 1 calc R . . C8 C 0.8308(3) 0.83977(19) 0.2323(2) 0.0305(10) Uani 1 1 d . . . C9 C 0.8427(4) 0.8971(2) 0.1917(2) 0.0420(11) Uani 1 1 d . . . H9 H 0.8163 0.8962 0.1448 0.05 Uiso 1 1 calc R . . C10 C 0.8930(4) 0.9562(2) 0.2189(3) 0.0521(13) Uani 1 1 d . . . H10 H 0.9001 0.9954 0.1906 0.062 Uiso 1 1 calc R . . C11 C 0.9322(4) 0.9578(3) 0.2864(3) 0.0602(14) Uani 1 1 d . . . H11 H 0.9645 0.9984 0.3053 0.072 Uiso 1 1 calc R . . C12 C 0.9247(5) 0.9005(3) 0.3266(3) 0.0676(16) Uani 1 1 d . . . H12 H 0.9551 0.9009 0.3728 0.081 Uiso 1 1 calc R . . C13 C 0.8728(4) 0.8418(2) 0.3000(2) 0.0492(12) Uani 1 1 d . . . H13 H 0.8661 0.8028 0.3285 0.059 Uiso 1 1 calc R . . C14 C 0.8985(3) 0.5779(2) 0.13710(19) 0.0306(10) Uani 1 1 d . . . C15 C 0.8405(4) 0.5216(2) 0.1134(3) 0.0587(14) Uani 1 1 d . . . H15 H 0.7926 0.5254 0.0732 0.07 Uiso 1 1 calc R . . C16 C 0.8505(5) 0.4587(2) 0.1476(3) 0.0678(16) Uani 1 1 d . . . H16 H 0.8103 0.42 0.1302 0.081 Uiso 1 1 calc R . . C17 C 0.9182(4) 0.4527(2) 0.2058(2) 0.0465(12) Uani 1 1 d . . . H17 H 0.9234 0.4104 0.2299 0.056 Uiso 1 1 calc R . . C18 C 0.9784(4) 0.5078(2) 0.2294(2) 0.0387(11) Uani 1 1 d . . . H18 H 1.0265 0.5036 0.2695 0.046 Uiso 1 1 calc R . . C19 C 0.9696(3) 0.5702(2) 0.19472(19) 0.0327(10) Uani 1 1 d . . . H19 H 1.0131 0.6079 0.2109 0.039 Uiso 1 1 calc R . . C20 C 1.0316(3) 0.6657(2) 0.06810(19) 0.0335(10) Uani 1 1 d . . . C21 C 1.0875(3) 0.7276(2) 0.0655(2) 0.0406(11) Uani 1 1 d . . . H21 H 1.0531 0.7684 0.0795 0.049 Uiso 1 1 calc R . . C22 C 1.1928(4) 0.7315(3) 0.0428(2) 0.0538(13) Uani 1 1 d . . . H22 H 1.2296 0.7743 0.0416 0.065 Uiso 1 1 calc R . . C23 C 1.2422(4) 0.6732(3) 0.0225(2) 0.0599(15) Uani 1 1 d . . . H23 H 1.3137 0.6757 0.0068 0.072 Uiso 1 1 calc R . . C24 C 1.1909(4) 0.6118(3) 0.0243(2) 0.0610(15) Uani 1 1 d . . . H24 H 1.2263 0.5716 0.0096 0.073 Uiso 1 1 calc R . . C25 C 1.0848(4) 0.6076(2) 0.0480(2) 0.0497(12) Uani 1 1 d . . . H25 H 1.0498 0.5643 0.0501 0.06 Uiso 1 1 calc R . . C26 C 0.5575(3) 0.7865(2) 0.15310(18) 0.0294(9) Uani 1 1 d . . . C27 C 0.4882(3) 0.7352(2) 0.1758(2) 0.0312(9) Uani 1 1 d . . . C28 C 0.3805(4) 0.7527(2) 0.1897(2) 0.0412(11) Uani 1 1 d . . . H28 H 0.3347 0.718 0.2063 0.049 Uiso 1 1 calc R . . C29 C 0.3387(3) 0.8174(2) 0.1805(2) 0.0398(11) Uani 1 1 d . . . C30 C 0.4072(3) 0.8665(2) 0.1547(2) 0.0386(11) Uani 1 1 d . . . H30 H 0.3791 0.9114 0.1464 0.046 Uiso 1 1 calc R . . C31 C 0.5152(3) 0.8530(2) 0.14063(19) 0.0315(10) Uani 1 1 d . . . C32 C 0.5214(4) 0.6608(2) 0.1829(2) 0.0422(11) Uani 1 1 d . . . H32A H 0.5961 0.6552 0.1689 0.063 Uiso 1 1 calc R . . H32B H 0.4712 0.6325 0.1536 0.063 Uiso 1 1 calc R . . H32C H 0.5185 0.6465 0.2308 0.063 Uiso 1 1 calc R . . C33 C 0.2222(4) 0.8348(3) 0.1952(3) 0.0579(14) Uani 1 1 d . . . H33A H 0.2083 0.8834 0.1854 0.087 Uiso 0.5 1 calc PR . . H33B H 0.2117 0.8256 0.2436 0.087 Uiso 0.5 1 calc PR . . H33C H 0.1714 0.8067 0.1662 0.087 Uiso 0.5 1 calc PR . . H33D H 0.1859 0.7937 0.2114 0.087 Uiso 0.5 1 calc PR . . H33E H 0.1826 0.8516 0.1532 0.087 Uiso 0.5 1 calc PR . . H33F H 0.2229 0.8704 0.2307 0.087 Uiso 0.5 1 calc PR . . C34 C 0.5808(4) 0.9094(2) 0.1114(2) 0.0422(11) Uani 1 1 d . . . H34A H 0.5315 0.9456 0.0933 0.063 Uiso 1 1 calc R . . H34B H 0.6222 0.8911 0.0743 0.063 Uiso 1 1 calc R . . H34C H 0.6317 0.9283 0.1475 0.063 Uiso 1 1 calc R . . C35 C 0.7715(3) 0.62522(18) -0.02330(19) 0.0274(9) Uani 1 1 d . . . C36 C 0.8347(3) 0.62929(19) -0.08033(19) 0.0280(9) Uani 1 1 d . . . C37 C 0.8141(3) 0.5836(2) -0.1342(2) 0.0352(10) Uani 1 1 d . . . H37 H 0.8579 0.5862 -0.1723 0.042 Uiso 1 1 calc R . . C38 C 0.7325(3) 0.5345(2) -0.1346(2) 0.0364(10) Uani 1 1 d . . . C39 C 0.6648(3) 0.5355(2) -0.0804(2) 0.0347(10) Uani 1 1 d . . . H39 H 0.605 0.5045 -0.081 0.042 Uiso 1 1 calc R . . C40 C 0.6815(3) 0.58021(19) -0.02555(19) 0.0293(9) Uani 1 1 d . . . C41 C 0.9195(3) 0.6843(2) -0.0878(2) 0.0379(11) Uani 1 1 d . . . H41A H 0.9017 0.7244 -0.0605 0.057 Uiso 1 1 calc R . . H41B H 0.9202 0.6975 -0.1362 0.057 Uiso 1 1 calc R . . H41C H 0.9918 0.6668 -0.0717 0.057 Uiso 1 1 calc R . . C42 C 0.7174(4) 0.4826(3) -0.1922(2) 0.0552(14) Uani 1 1 d . . . H42A H 0.7732 0.4901 -0.225 0.083 Uiso 0.5 1 calc PR . . H42B H 0.6445 0.4881 -0.2156 0.083 Uiso 0.5 1 calc PR . . H42C H 0.7249 0.4362 -0.1732 0.083 Uiso 0.5 1 calc PR . . H42D H 0.6552 0.4528 -0.1842 0.083 Uiso 0.5 1 calc PR . . H42E H 0.7839 0.4548 -0.1937 0.083 Uiso 0.5 1 calc PR . . H42F H 0.7035 0.5067 -0.236 0.083 Uiso 0.5 1 calc PR . . C43 C 0.6015(4) 0.5800(2) 0.0301(2) 0.0421(11) Uani 1 1 d . . . H43A H 0.5266 0.5836 0.0091 0.063 Uiso 1 1 calc R . . H43B H 0.6167 0.619 0.0609 0.063 Uiso 1 1 calc R . . H43C H 0.6093 0.5373 0.0563 0.063 Uiso 1 1 calc R . . C44 C 0.5218(4) 0.7621(3) -0.0354(2) 0.0541(13) Uani 1 1 d . . . H44A H 0.5542 0.7163 -0.0298 0.081 Uiso 1 1 calc R . . H44B H 0.4534 0.7591 -0.0644 0.081 Uiso 1 1 calc R . . H44C H 0.5066 0.7804 0.0097 0.081 Uiso 1 1 calc R . . C45 C 0.5443(4) 0.9017(2) -0.0980(3) 0.0642(15) Uani 1 1 d . . . H45A H 0.5181 0.9216 -0.0561 0.096 Uiso 1 1 calc R . . H45B H 0.4818 0.8922 -0.1307 0.096 Uiso 1 1 calc R . . H45C H 0.5938 0.9341 -0.1184 0.096 Uiso 1 1 calc R . . C46 C 0.6466(5) 0.7785(3) -0.1597(2) 0.0665(15) Uani 1 1 d . . . H46A H 0.6964 0.8074 -0.1842 0.1 Uiso 1 1 calc R . . H46B H 0.5776 0.7729 -0.1876 0.1 Uiso 1 1 calc R . . H46C H 0.6803 0.7336 -0.1508 0.1 Uiso 1 1 calc R . . C47 C 0.8539(4) 0.9118(3) -0.1252(2) 0.0635(15) Uani 1 1 d . . . H47A H 0.8814 0.8689 -0.1436 0.095 Uiso 1 1 calc R . . H47B H 0.9095 0.9477 -0.1277 0.095 Uiso 1 1 calc R . . H47C H 0.787 0.9257 -0.1522 0.095 Uiso 1 1 calc R . . C48 C 0.9576(4) 0.8854(3) 0.0148(3) 0.0550(13) Uani 1 1 d . . . H48A H 0.9464 0.8773 0.0633 0.083 Uiso 1 1 calc R . . H48B H 1.0031 0.9263 0.0106 0.083 Uiso 1 1 calc R . . H48C H 0.9942 0.8457 -0.004 0.083 Uiso 1 1 calc R . . C49 C 0.7707(4) 0.9835(2) -0.0029(3) 0.0593(14) Uani 1 1 d . . . H49A H 0.6962 0.9912 -0.0231 0.089 Uiso 1 1 calc R . . H49B H 0.8186 1.0204 -0.0169 0.089 Uiso 1 1 calc R . . H49C H 0.7702 0.983 0.0472 0.089 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 Co 0.0356(3) 0.0222(3) 0.0245(3) 0.0012(2) 0.0090(2) 0.0005(2) P1 0.0362(6) 0.0217(6) 0.0244(6) -0.0010(4) 0.0085(5) 0.0007(5) P2 0.0357(6) 0.0223(6) 0.0257(6) -0.0016(4) 0.0074(5) 0.0015(5) Si1 0.0483(8) 0.0347(7) 0.0312(7) 0.0028(5) 0.0025(6) -0.0002(6) Si2 0.0454(8) 0.0334(7) 0.0380(7) 0.0087(5) 0.0137(6) -0.0052(6) N1 0.0356(19) 0.0204(18) 0.0285(18) -0.0004(14) 0.0103(15) 0.0012(14) N2 0.038(2) 0.0223(18) 0.0300(18) 0.0009(14) 0.0101(15) -0.0013(15) N3 0.040(2) 0.0251(18) 0.0306(19) 0.0027(15) 0.0107(15) 0.0015(15) C1 0.035(2) 0.027(2) 0.029(2) -0.0064(18) 0.0120(18) -0.0056(18) C2 0.034(2) 0.029(2) 0.024(2) 0.0001(18) 0.0100(18) 0.0013(18) C3 0.047(3) 0.028(2) 0.040(3) 0.004(2) 0.017(2) 0.004(2) C4 0.055(3) 0.033(3) 0.048(3) 0.013(2) 0.019(2) 0.007(2) C5 0.058(3) 0.048(3) 0.039(3) 0.015(2) 0.026(2) 0.011(2) C6 0.059(3) 0.053(3) 0.033(3) 0.009(2) 0.026(2) 0.017(3) C7 0.054(3) 0.033(2) 0.032(2) 0.003(2) 0.012(2) 0.011(2) C8 0.034(2) 0.022(2) 0.036(2) -0.0034(19) 0.0076(19) 0.0026(18) C9 0.047(3) 0.034(3) 0.045(3) -0.001(2) 0.008(2) -0.003(2) C10 0.056(3) 0.033(3) 0.068(4) 0.007(2) 0.007(3) -0.005(2) C11 0.072(4) 0.041(3) 0.066(4) -0.017(3) -0.007(3) -0.016(3) C12 0.094(4) 0.051(3) 0.054(3) -0.005(3) -0.019(3) -0.022(3) C13 0.069(3) 0.033(3) 0.043(3) -0.002(2) -0.011(2) -0.005(2) C14 0.040(2) 0.027(2) 0.026(2) 0.0027(18) 0.0080(19) 0.0037(19) C15 0.071(4) 0.034(3) 0.066(3) 0.013(2) -0.027(3) -0.014(3) C16 0.088(4) 0.032(3) 0.079(4) 0.018(3) -0.025(3) -0.022(3) C17 0.065(3) 0.036(3) 0.040(3) 0.012(2) 0.010(2) 0.006(2) C18 0.050(3) 0.038(3) 0.029(2) -0.001(2) 0.007(2) 0.009(2) C19 0.041(3) 0.030(2) 0.028(2) -0.0014(19) 0.011(2) -0.0007(19) C20 0.041(3) 0.040(3) 0.020(2) 0.0010(18) 0.0078(19) 0.005(2) C21 0.039(3) 0.047(3) 0.037(2) -0.006(2) 0.012(2) 0.000(2) C22 0.042(3) 0.075(4) 0.046(3) -0.008(3) 0.011(2) -0.010(3) C23 0.045(3) 0.091(5) 0.045(3) 0.015(3) 0.017(2) 0.007(3) C24 0.064(4) 0.072(4) 0.051(3) 0.011(3) 0.029(3) 0.041(3) C25 0.066(3) 0.042(3) 0.044(3) 0.002(2) 0.020(2) 0.013(2) C26 0.036(2) 0.034(2) 0.019(2) -0.0023(17) 0.0052(18) 0.0019(19) C27 0.034(2) 0.033(2) 0.028(2) -0.0014(19) 0.0091(18) -0.0056(19) C28 0.041(3) 0.049(3) 0.034(2) -0.001(2) 0.012(2) -0.010(2) C29 0.036(3) 0.054(3) 0.029(2) -0.009(2) 0.003(2) 0.002(2) C30 0.045(3) 0.039(3) 0.032(2) -0.008(2) 0.003(2) 0.009(2) C31 0.034(2) 0.037(3) 0.023(2) -0.0056(18) 0.0059(18) 0.0000(19) C32 0.053(3) 0.033(2) 0.042(3) 0.000(2) 0.015(2) -0.012(2) C33 0.037(3) 0.083(4) 0.054(3) -0.013(3) 0.011(2) 0.010(3) C34 0.047(3) 0.033(3) 0.048(3) 0.000(2) 0.013(2) 0.007(2) C35 0.037(2) 0.020(2) 0.025(2) -0.0028(17) 0.0034(18) 0.0014(18) C36 0.033(2) 0.025(2) 0.026(2) -0.0023(18) 0.0069(18) 0.0006(18) C37 0.042(3) 0.038(3) 0.028(2) -0.0040(19) 0.0133(19) 0.001(2) C38 0.042(3) 0.034(2) 0.033(2) -0.0085(19) 0.007(2) -0.002(2) C39 0.034(2) 0.031(2) 0.039(3) -0.006(2) 0.005(2) -0.0036(19) C40 0.032(2) 0.025(2) 0.031(2) 0.0018(18) 0.0088(18) 0.0012(18) C41 0.047(3) 0.038(3) 0.029(2) -0.0026(19) 0.010(2) -0.008(2) C42 0.057(3) 0.061(3) 0.049(3) -0.026(3) 0.015(2) -0.012(3) C43 0.046(3) 0.044(3) 0.039(3) -0.005(2) 0.016(2) -0.010(2) C44 0.054(3) 0.061(3) 0.047(3) -0.001(2) -0.001(2) -0.016(3) C45 0.065(4) 0.052(3) 0.073(4) 0.013(3) -0.016(3) 0.005(3) C46 0.074(4) 0.081(4) 0.044(3) -0.011(3) 0.001(3) -0.011(3) C47 0.076(4) 0.070(4) 0.048(3) 0.019(3) 0.023(3) -0.015(3) C48 0.050(3) 0.056(3) 0.061(3) 0.007(3) 0.016(3) -0.010(2) C49 0.063(3) 0.034(3) 0.083(4) 0.002(3) 0.017(3) -0.011(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N3 1.934(3) . ? Co N1 1.996(3) . ? Co N2 1.997(3) . ? P1 N1 1.616(3) . ? P1 C1 1.729(4) . ? P1 C2 1.810(4) . ? P1 C8 1.821(4) . ? P2 N2 1.618(3) . ? P2 C1 1.735(4) . ? P2 C20 1.822(4) . ? P2 C14 1.828(4) . ? Si1 N3 1.714(3) . ? Si1 C44 1.866(5) . ? Si1 C46 1.868(5) . ? Si1 C45 1.872(5) . ? Si2 N3 1.709(3) . ? Si2 C48 1.861(5) . ? Si2 C47 1.877(5) . ? Si2 C49 1.884(5) . ? N1 C26 1.443(5) . ? N2 C35 1.446(5) . ? C2 C3 1.384(5) . ? C2 C7 1.401(5) . ? C3 C4 1.378(6) . ? C4 C5 1.367(6) . ? C5 C6 1.371(6) . ? C6 C7 1.384(6) . ? C8 C13 1.385(6) . ? C8 C9 1.385(6) . ? C9 C10 1.394(6) . ? C10 C11 1.373(7) . ? C11 C12 1.372(7) . ? C12 C13 1.393(6) . ? C14 C15 1.371(6) . ? C14 C19 1.382(5) . ? C15 C16 1.399(6) . ? C16 C17 1.365(6) . ? C17 C18 1.365(6) . ? C18 C19 1.393(6) . ? C20 C25 1.380(6) . ? C20 C21 1.391(6) . ? C21 C22 1.395(6) . ? C22 C23 1.360(7) . ? C23 C24 1.355(7) . ? C24 C25 1.413(6) . ? C26 C27 1.404(5) . ? C26 C31 1.413(5) . ? C27 C28 1.407(6) . ? C27 C32 1.512(5) . ? C28 C29 1.369(6) . ? C29 C30 1.392(6) . ? C29 C33 1.514(6) . ? C30 C31 1.396(5) . ? C31 C34 1.499(6) . ? C35 C36 1.402(5) . ? C35 C40 1.408(5) . ? C36 C37 1.388(5) . ? C36 C41 1.509(5) . ? C37 C38 1.384(6) . ? C38 C39 1.391(5) . ? C38 C42 1.514(6) . ? C39 C40 1.385(5) . ? C40 C43 1.514(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 N3 Co N1 126.00(13) . . ? N3 Co N2 122.06(13) . . ? N1 Co N2 110.87(12) . . ? N1 P1 C1 106.65(17) . . ? N1 P1 C2 111.94(17) . . ? C1 P1 C2 117.90(18) . . ? N1 P1 C8 116.62(17) . . ? C1 P1 C8 101.98(18) . . ? C2 P1 C8 101.76(18) . . ? N2 P2 C1 105.34(18) . . ? N2 P2 C20 116.92(17) . . ? C1 P2 C20 105.88(19) . . ? N2 P2 C14 114.30(17) . . ? C1 P2 C14 115.31(18) . . ? C20 P2 C14 99.16(18) . . ? N3 Si1 C44 110.38(19) . . ? N3 Si1 C46 113.4(2) . . ? C44 Si1 C46 105.7(2) . . ? N3 Si1 C45 112.9(2) . . ? C44 Si1 C45 107.1(2) . . ? C46 Si1 C45 106.8(3) . . ? N3 Si2 C48 112.25(19) . . ? N3 Si2 C47 112.8(2) . . ? C48 Si2 C47 105.7(2) . . ? N3 Si2 C49 113.53(19) . . ? C48 Si2 C49 105.7(2) . . ? C47 Si2 C49 106.2(2) . . ? C26 N1 P1 126.0(2) . . ? C26 N1 Co 132.2(2) . . ? P1 N1 Co 101.73(16) . . ? C35 N2 P2 127.3(3) . . ? C35 N2 Co 128.0(2) . . ? P2 N2 Co 102.97(16) . . ? Si2 N3 Si1 122.30(19) . . ? Si2 N3 Co 127.99(19) . . ? Si1 N3 Co 109.59(16) . . ? P1 C1 P2 133.5(2) . . ? C3 C2 C7 118.0(4) . . ? C3 C2 P1 121.2(3) . . ? C7 C2 P1 120.8(3) . . ? C4 C3 C2 121.3(4) . . ? C5 C4 C3 119.9(4) . . ? C4 C5 C6 120.3(4) . . ? C5 C6 C7 120.3(4) . . ? C6 C7 C2 120.2(4) . . ? C13 C8 C9 118.4(4) . . ? C13 C8 P1 122.2(3) . . ? C9 C8 P1 119.2(3) . . ? C8 C9 C10 120.8(4) . . ? C11 C10 C9 120.0(5) . . ? C12 C11 C10 119.9(4) . . ? C11 C12 C13 120.1(5) . . ? C8 C13 C12 120.7(4) . . ? C15 C14 C19 118.0(4) . . ? C15 C14 P2 124.0(3) . . ? C19 C14 P2 117.9(3) . . ? C14 C15 C16 121.1(4) . . ? C17 C16 C15 120.0(4) . . ? C18 C17 C16 119.7(4) . . ? C17 C18 C19 120.2(4) . . ? C14 C19 C18 120.9(4) . . ? C25 C20 C21 117.3(4) . . ? C25 C20 P2 121.1(3) . . ? C21 C20 P2 121.5(3) . . ? C20 C21 C22 121.8(4) . . ? C23 C22 C21 119.2(5) . . ? C24 C23 C22 121.0(5) . . ? C23 C24 C25 119.9(5) . . ? C20 C25 C24 120.6(5) . . ? C27 C26 C31 119.1(4) . . ? C27 C26 N1 121.9(3) . . ? C31 C26 N1 118.9(3) . . ? C26 C27 C28 119.0(4) . . ? C26 C27 C32 123.2(4) . . ? C28 C27 C32 117.7(4) . . ? C29 C28 C27 123.0(4) . . ? C28 C29 C30 117.0(4) . . ? C28 C29 C33 122.0(4) . . ? C30 C29 C33 120.9(4) . . ? C29 C30 C31 123.1(4) . . ? C30 C31 C26 118.7(4) . . ? C30 C31 C34 118.6(4) . . ? C26 C31 C34 122.6(3) . . ? C36 C35 C40 119.0(3) . . ? C36 C35 N2 120.8(3) . . ? C40 C35 N2 120.1(3) . . ? C37 C36 C35 119.0(4) . . ? C37 C36 C41 118.2(3) . . ? C35 C36 C41 122.7(3) . . ? C38 C37 C36 122.8(4) . . ? C37 C38 C39 117.0(4) . . ? C37 C38 C42 121.2(4) . . ? C39 C38 C42 121.8(4) . . ? C40 C39 C38 122.4(4) . . ? C39 C40 C35 119.3(3) . . ? C39 C40 C43 119.1(4) . . ? C35 C40 C43 121.6(3) . . ? #===END data_may1302 _database_code_CSD 191082 _audit_creation_date 2002-05-13T10:53:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Fe(OCPh3)(MesNPPh2CHPPh2NMes)] _chemical_formula_sum 'C62 H58 Fe N2 O P2' _chemical_formula_weight 964.89 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4976(2) _cell_length_b 12.7168(2) _cell_length_c 19.7847(4) _cell_angle_alpha 92.801(1) _cell_angle_beta 92.638(1) _cell_angle_gamma 107.006(1) _cell_volume 2517.63(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14433 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.918 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_unetI/netI 0.0771 _diffrn_reflns_number 24791 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 11383 _reflns_number_gt 7910 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.7152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding; torsion refined for o-methyls' _refine_ls_extinction_method none _refine_ls_number_reflns 11383 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.489 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.006 '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' 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 Fe Fe 0.56139(3) 0.71499(3) 0.751070(18) 0.02099(10) Uani 1 1 d . . . P1 P 0.81264(6) 0.80772(5) 0.70738(3) 0.02020(14) Uani 1 1 d . . . P2 P 0.72038(6) 0.57468(5) 0.76514(3) 0.02058(14) Uani 1 1 d . . . O O 0.44792(16) 0.74738(14) 0.81264(9) 0.0279(4) Uani 1 1 d . . . N1 N 0.66705(19) 0.80428(16) 0.67549(10) 0.0224(4) Uani 1 1 d . . . N2 N 0.57421(19) 0.55443(15) 0.72947(10) 0.0220(4) Uani 1 1 d . . . C1 C 0.7868(2) 0.71722(19) 0.77196(13) 0.0212(5) Uani 1 1 d . . . H1 H 0.831(3) 0.746(2) 0.8132(15) 0.040(8) Uiso 1 1 d . . . C2 C 0.9023(2) 0.9378(2) 0.75334(13) 0.0261(6) Uani 1 1 d . . . C3 C 0.8425(3) 1.0225(2) 0.75636(14) 0.0344(6) Uani 1 1 d . . . H3 H 0.7596 1.0132 0.7318 0.041 Uiso 1 1 calc R . . C4 C 0.9035(4) 1.1209(2) 0.79514(16) 0.0485(8) Uani 1 1 d . . . C5 C 1.0253(4) 1.1327(3) 0.82979(16) 0.0536(9) Uani 1 1 d . . . H5 H 1.0682 1.1996 0.8558 0.064 Uiso 1 1 calc R . . C6 C 1.0857(3) 1.0497(3) 0.82737(15) 0.0445(8) Uani 1 1 d . . . H6 H 1.1695 1.0598 0.8512 0.053 Uiso 1 1 calc R . . C7 C 1.0234(3) 0.9518(2) 0.79003(13) 0.0332(6) Uani 1 1 d . . . H7 H 1.0634 0.8938 0.7894 0.04 Uiso 1 1 calc R . . C8 C 0.9150(2) 0.7808(2) 0.64086(12) 0.0237(5) Uani 1 1 d . . . C9 C 1.0531(2) 0.8287(2) 0.64118(14) 0.0300(6) Uani 1 1 d . . . H9 H 1.0987 0.8793 0.6775 0.036 Uiso 1 1 calc R . . C10 C 1.1238(3) 0.8025(3) 0.58879(15) 0.0398(7) Uani 1 1 d . . . H10 H 1.2175 0.8357 0.5893 0.048 Uiso 1 1 calc R . . C11 C 1.0589(3) 0.7285(3) 0.53579(16) 0.0477(8) Uani 1 1 d . . . H11 H 1.108 0.7104 0.5001 0.057 Uiso 1 1 calc R . . C12 C 0.9222(3) 0.6808(3) 0.53494(16) 0.0458(8) Uani 1 1 d . . . H12 H 0.8769 0.6302 0.4986 0.055 Uiso 1 1 calc R . . C13 C 0.8515(3) 0.7072(2) 0.58731(14) 0.0325(6) Uani 1 1 d . . . H13 H 0.7577 0.6742 0.5865 0.039 Uiso 1 1 calc R . . C14 C 0.8262(2) 0.5035(2) 0.72264(13) 0.0276(6) Uani 1 1 d . . . H14 H 0.7676 0.5397 0.7417 0.033 Uiso 1 1 calc R . . C15 C 0.9605(3) 0.5591(2) 0.72045(15) 0.0355(7) Uani 1 1 d . . . H15 H 0.9945 0.6333 0.7385 0.043 Uiso 1 1 calc R . . C16 C 1.0455(3) 0.5063(3) 0.69186(18) 0.0520(9) Uani 1 1 d . . . H16 H 1.1379 0.5443 0.6907 0.062 Uiso 1 1 calc R . . C17 C 0.9970(4) 0.4000(3) 0.66531(19) 0.0610(10) Uani 1 1 d . . . H17 H 1.0551 0.3648 0.6448 0.073 Uiso 1 1 calc R . . C18 C 0.8640(4) 0.3439(3) 0.66833(19) 0.0620(11) Uani 1 1 d . . . H18 H 0.831 0.2694 0.6507 0.074 Uiso 1 1 calc R . . C19 C 0.7775(3) 0.3954(2) 0.69706(16) 0.0446(8) Uani 1 1 d . . . H19 H 0.6856 0.3566 0.699 0.054 Uiso 1 1 calc R . . C20 C 0.7235(2) 0.5307(2) 0.85128(13) 0.0256(5) Uani 1 1 d . . . C21 C 0.6744(3) 0.5849(2) 0.90219(14) 0.0346(6) Uani 1 1 d . . . H21 H 0.6443 0.6462 0.8919 0.042 Uiso 1 1 calc R . . C22 C 0.6688(3) 0.5505(2) 0.96791(15) 0.0443(8) Uani 1 1 d . . . H22 H 0.6344 0.5876 1.0021 0.053 Uiso 1 1 calc R . . C23 C 0.7136(3) 0.4622(3) 0.98314(16) 0.0508(9) Uani 1 1 d . . . H23 H 0.7101 0.4385 1.028 0.061 Uiso 1 1 calc R . . C24 C 0.7630(3) 0.4086(3) 0.93410(17) 0.0503(8) Uani 1 1 d . . . H24 H 0.7939 0.3481 0.9452 0.06 Uiso 1 1 calc R . . C25 C 0.7684(3) 0.4417(2) 0.86822(15) 0.0361(7) Uani 1 1 d . . . H25 H 0.8028 0.4036 0.8345 0.043 Uiso 1 1 calc R . . C26 C 0.6213(2) 0.82679(19) 0.61068(12) 0.0226(5) Uani 1 1 d . . . C27 C 0.4879(2) 0.76714(19) 0.58871(12) 0.0232(5) Uani 1 1 d . . . C28 C 0.4354(2) 0.7828(2) 0.52581(13) 0.0271(6) Uani 1 1 d . . . H28 H 0.3465 0.7407 0.5118 0.033 Uiso 1 1 calc R . . C29 C 0.5067(3) 0.8569(2) 0.48264(13) 0.0285(6) Uani 1 1 d . . . C30 C 0.6346(3) 0.9167(2) 0.50494(13) 0.0293(6) Uani 1 1 d . . . H30 H 0.6852 0.9689 0.4762 0.035 Uiso 1 1 calc R . . C31 C 0.6938(2) 0.9048(2) 0.56744(13) 0.0260(5) Uani 1 1 d . . . C32 C 0.3994(2) 0.6866(2) 0.63249(14) 0.0300(6) Uani 1 1 d . . . H32A H 0.3133 0.6512 0.6077 0.045 Uiso 1 1 calc R . . H32B H 0.3851 0.7258 0.674 0.045 Uiso 1 1 calc R . . H32C H 0.4421 0.6304 0.6443 0.045 Uiso 1 1 calc R . . C33 C 0.4472(3) 0.8708(3) 0.41376(14) 0.0429(7) Uani 1 1 d . . . H33A H 0.3558 0.8213 0.4072 0.064 Uiso 0.5 1 calc PR . . H33B H 0.5013 0.8529 0.3784 0.064 Uiso 0.5 1 calc PR . . H33C H 0.4459 0.9472 0.411 0.064 Uiso 0.5 1 calc PR . . H33D H 0.5128 0.9263 0.3906 0.064 Uiso 0.5 1 calc PR . . H33E H 0.3674 0.8947 0.4194 0.064 Uiso 0.5 1 calc PR . . H33F H 0.4228 0.8004 0.3867 0.064 Uiso 0.5 1 calc PR . . C34 C 0.8324(3) 0.9820(2) 0.58396(16) 0.0407(7) Uani 1 1 d . . . H34A H 0.8978 0.951 0.5633 0.061 Uiso 1 1 calc R . . H34B H 0.8507 0.9913 0.6333 0.061 Uiso 1 1 calc R . . H34C H 0.8387 1.0536 0.566 0.061 Uiso 1 1 calc R . . C35 C 0.4732(2) 0.45494(19) 0.70591(13) 0.0228(5) Uani 1 1 d . . . C36 C 0.3734(2) 0.4026(2) 0.74853(13) 0.0270(6) Uani 1 1 d . . . C37 C 0.2712(3) 0.3104(2) 0.72240(15) 0.0340(6) Uani 1 1 d . . . H37 H 0.2044 0.2749 0.7514 0.041 Uiso 1 1 calc R . . C38 C 0.2631(2) 0.2685(2) 0.65592(16) 0.0331(7) Uani 1 1 d . . . C39 C 0.3600(3) 0.3225(2) 0.61429(15) 0.0327(6) Uani 1 1 d . . . H39 H 0.3551 0.2958 0.5683 0.039 Uiso 1 1 calc R . . C40 C 0.4647(2) 0.4150(2) 0.63751(13) 0.0262(6) Uani 1 1 d . . . C41 C 0.3742(3) 0.4437(2) 0.82116(14) 0.0406(7) Uani 1 1 d . . . H41A H 0.2855 0.4129 0.8381 0.061 Uiso 1 1 calc R . . H41B H 0.3974 0.5243 0.8241 0.061 Uiso 1 1 calc R . . H41C H 0.4401 0.4207 0.8487 0.061 Uiso 1 1 calc R . . C42 C 0.1512(3) 0.1671(2) 0.62976(18) 0.0476(8) Uani 1 1 d . . . H42A H 0.1621 0.1495 0.582 0.071 Uiso 0.5 1 calc PR . . H42B H 0.0651 0.1816 0.634 0.071 Uiso 0.5 1 calc PR . . H42C H 0.154 0.1047 0.6564 0.071 Uiso 0.5 1 calc PR . . H42D H 0.0921 0.141 0.6663 0.071 Uiso 0.5 1 calc PR . . H42E H 0.1891 0.1089 0.6142 0.071 Uiso 0.5 1 calc PR . . H42F H 0.1001 0.1858 0.5919 0.071 Uiso 0.5 1 calc PR . . C43 C 0.5631(3) 0.4715(2) 0.58826(14) 0.0359(7) Uani 1 1 d . . . H43A H 0.5486 0.4258 0.5456 0.054 Uiso 1 1 calc R . . H43B H 0.6541 0.4822 0.6074 0.054 Uiso 1 1 calc R . . H43C H 0.5508 0.5432 0.5796 0.054 Uiso 1 1 calc R . . C44 C 0.4435(2) 0.82969(19) 0.86171(12) 0.0230(5) Uani 1 1 d . . . C45 C 0.4551(2) 0.9394(2) 0.82873(12) 0.0245(5) Uani 1 1 d . . . C46 C 0.3877(3) 0.9356(2) 0.76611(14) 0.0359(7) Uani 1 1 d . . . H46 H 0.339 0.8664 0.7442 0.043 Uiso 1 1 calc R . . C47 C 0.3908(3) 1.0316(3) 0.73540(16) 0.0459(8) Uani 1 1 d . . . H47 H 0.3436 1.0278 0.6928 0.055 Uiso 1 1 calc R . . C48 C 0.4616(3) 1.1327(3) 0.76606(17) 0.0456(8) Uani 1 1 d . . . H48 H 0.4642 1.1983 0.7445 0.055 Uiso 1 1 calc R . . C49 C 0.5283(3) 1.1379(2) 0.82795(16) 0.0409(7) Uani 1 1 d . . . H49 H 0.5773 1.2074 0.8492 0.049 Uiso 1 1 calc R . . C50 C 0.5245(3) 1.0415(2) 0.85994(14) 0.0332(6) Uani 1 1 d . . . H50 H 0.5697 1.046 0.9032 0.04 Uiso 1 1 calc R . . C51 C 0.5582(2) 0.84193(19) 0.91556(13) 0.0238(5) Uani 1 1 d . . . C52 C 0.6887(2) 0.8842(2) 0.89552(13) 0.0286(6) Uani 1 1 d . . . H52 H 0.7024 0.9096 0.8513 0.034 Uiso 1 1 calc R . . C53 C 0.7980(3) 0.8895(2) 0.93880(14) 0.0347(7) Uani 1 1 d . . . H53 H 0.8857 0.9171 0.924 0.042 Uiso 1 1 calc R . . C54 C 0.7796(3) 0.8547(2) 1.00328(15) 0.0401(7) Uani 1 1 d . . . H54 H 0.8546 0.859 1.0332 0.048 Uiso 1 1 calc R . . C55 C 0.6515(3) 0.8133(2) 1.02453(14) 0.0372(7) Uani 1 1 d . . . H55 H 0.6386 0.7893 1.0691 0.045 Uiso 1 1 calc R . . C56 C 0.5420(3) 0.8068(2) 0.98063(13) 0.0303(6) Uani 1 1 d . . . H56 H 0.4545 0.7778 0.9955 0.036 Uiso 1 1 calc R . . C57 C 0.3057(2) 0.7962(2) 0.89232(13) 0.0242(5) Uani 1 1 d . . . C58 C 0.2127(3) 0.6968(2) 0.87154(14) 0.0311(6) Uani 1 1 d . . . H58 H 0.2346 0.6485 0.8389 0.037 Uiso 1 1 calc R . . C59 C 0.0873(3) 0.6665(2) 0.89791(16) 0.0417(7) Uani 1 1 d . . . H59 H 0.0245 0.5979 0.8831 0.05 Uiso 1 1 calc R . . C60 C 0.0537(3) 0.7351(3) 0.94514(16) 0.0427(7) Uani 1 1 d . . . H60 H -0.0317 0.714 0.9633 0.051 Uiso 1 1 calc R . . C61 C 0.1447(3) 0.8343(2) 0.96579(15) 0.0399(7) Uani 1 1 d . . . H61 H 0.1219 0.8822 0.9983 0.048 Uiso 1 1 calc R . . C62 C 0.2699(3) 0.8654(2) 0.93965(14) 0.0322(6) Uani 1 1 d . . . H62 H 0.3317 0.9346 0.9542 0.039 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 Fe 0.01882(18) 0.02007(19) 0.02441(19) 0.00098(14) 0.00507(14) 0.00579(14) P1 0.0167(3) 0.0184(3) 0.0238(3) 0.0022(2) 0.0023(3) 0.0023(2) P2 0.0187(3) 0.0182(3) 0.0253(3) 0.0013(2) 0.0028(3) 0.0060(2) O 0.0258(9) 0.0276(10) 0.0300(10) -0.0054(7) 0.0070(8) 0.0077(8) N1 0.0172(10) 0.0256(11) 0.0247(11) 0.0067(8) 0.0025(9) 0.0056(8) N2 0.0191(10) 0.0181(10) 0.0276(11) -0.0003(8) 0.0003(9) 0.0042(8) C1 0.0207(12) 0.0192(13) 0.0220(13) 0.0006(10) -0.0005(11) 0.0034(10) C2 0.0271(13) 0.0191(13) 0.0267(13) 0.0022(10) 0.0045(11) -0.0020(10) C3 0.0436(16) 0.0225(14) 0.0359(16) 0.0066(11) 0.0106(13) 0.0061(12) C4 0.072(2) 0.0270(16) 0.0400(18) -0.0005(13) 0.0135(17) 0.0035(15) C5 0.076(2) 0.0271(17) 0.0381(18) -0.0058(13) 0.0098(18) -0.0148(16) C6 0.0430(18) 0.0445(19) 0.0305(16) -0.0032(13) -0.0009(14) -0.0099(15) C7 0.0307(14) 0.0330(15) 0.0295(15) 0.0014(12) 0.0036(12) -0.0006(12) C8 0.0215(12) 0.0250(13) 0.0251(13) 0.0053(10) 0.0028(10) 0.0069(10) C9 0.0224(13) 0.0335(15) 0.0327(15) 0.0027(12) 0.0035(11) 0.0059(11) C10 0.0248(14) 0.0500(19) 0.0448(18) 0.0057(14) 0.0110(13) 0.0094(13) C11 0.0378(17) 0.071(2) 0.0384(18) -0.0032(16) 0.0138(14) 0.0213(16) C12 0.0387(17) 0.059(2) 0.0378(17) -0.0146(15) 0.0020(14) 0.0146(15) C13 0.0250(13) 0.0358(16) 0.0351(15) -0.0019(12) 0.0030(12) 0.0068(12) C14 0.0266(13) 0.0301(14) 0.0304(14) -0.0020(11) 0.0010(11) 0.0159(11) C15 0.0291(14) 0.0368(16) 0.0449(17) 0.0074(13) 0.0071(13) 0.0152(13) C16 0.0370(17) 0.065(2) 0.064(2) 0.0121(18) 0.0149(16) 0.0280(17) C17 0.053(2) 0.080(3) 0.066(2) -0.013(2) 0.0024(19) 0.049(2) C18 0.061(2) 0.059(2) 0.075(3) -0.0350(19) -0.024(2) 0.0415(19) C19 0.0369(16) 0.0409(18) 0.059(2) -0.0177(15) -0.0100(15) 0.0212(14) C20 0.0204(12) 0.0226(13) 0.0308(14) 0.0049(10) -0.0018(11) 0.0014(10) C21 0.0406(16) 0.0287(15) 0.0337(15) 0.0052(12) 0.0036(13) 0.0083(13) C22 0.060(2) 0.0376(18) 0.0288(16) 0.0043(13) 0.0060(15) 0.0032(15) C23 0.069(2) 0.0419(19) 0.0316(17) 0.0153(14) -0.0020(16) 0.0007(17) C24 0.057(2) 0.0394(18) 0.055(2) 0.0241(16) -0.0045(17) 0.0131(16) C25 0.0345(15) 0.0295(15) 0.0443(17) 0.0096(12) -0.0012(13) 0.0089(12) C26 0.0225(12) 0.0217(13) 0.0248(13) 0.0029(10) 0.0022(10) 0.0080(10) C27 0.0222(12) 0.0221(13) 0.0272(13) 0.0003(10) 0.0048(11) 0.0091(10) C28 0.0221(13) 0.0291(14) 0.0305(14) -0.0019(11) -0.0002(11) 0.0090(11) C29 0.0332(14) 0.0324(15) 0.0246(13) -0.0019(11) 0.0010(12) 0.0176(12) C30 0.0354(15) 0.0284(14) 0.0260(14) 0.0065(11) 0.0072(12) 0.0110(12) C31 0.0270(13) 0.0226(13) 0.0284(14) 0.0036(10) 0.0033(11) 0.0069(11) C32 0.0195(12) 0.0323(15) 0.0355(15) 0.0059(12) -0.0008(11) 0.0033(11) C33 0.0538(19) 0.0503(19) 0.0263(15) 0.0013(13) -0.0035(14) 0.0193(16) C34 0.0307(15) 0.0380(17) 0.0477(18) 0.0188(14) 0.0017(14) -0.0011(13) C35 0.0187(12) 0.0180(12) 0.0320(14) 0.0028(10) -0.0022(11) 0.0063(10) C36 0.0226(13) 0.0227(13) 0.0352(15) 0.0047(11) 0.0036(11) 0.0053(10) C37 0.0249(14) 0.0234(14) 0.0523(18) 0.0104(12) 0.0070(13) 0.0032(11) C38 0.0216(13) 0.0184(13) 0.0564(19) -0.0019(12) -0.0060(13) 0.0035(11) C39 0.0303(14) 0.0288(15) 0.0398(16) -0.0067(12) -0.0051(13) 0.0123(12) C40 0.0218(12) 0.0214(13) 0.0348(15) -0.0015(11) -0.0003(11) 0.0063(10) C41 0.0347(16) 0.0407(17) 0.0399(17) 0.0046(13) 0.0134(14) -0.0008(13) C42 0.0320(16) 0.0301(16) 0.072(2) -0.0059(15) -0.0068(16) -0.0019(13) C43 0.0367(16) 0.0356(16) 0.0329(15) -0.0049(12) 0.0031(13) 0.0079(13) C44 0.0213(12) 0.0217(13) 0.0259(13) -0.0004(10) 0.0062(10) 0.0059(10) C45 0.0213(12) 0.0280(14) 0.0262(13) 0.0034(10) 0.0089(11) 0.0087(11) C46 0.0323(15) 0.0391(17) 0.0355(16) 0.0062(13) 0.0009(13) 0.0090(13) C47 0.0413(17) 0.056(2) 0.0441(18) 0.0196(16) 0.0023(15) 0.0170(16) C48 0.0429(18) 0.0429(19) 0.060(2) 0.0275(16) 0.0194(16) 0.0201(15) C49 0.0435(17) 0.0251(15) 0.055(2) 0.0061(13) 0.0149(16) 0.0095(13) C50 0.0406(16) 0.0272(15) 0.0334(15) 0.0037(11) 0.0070(13) 0.0114(12) C51 0.0248(13) 0.0195(13) 0.0271(13) -0.0022(10) 0.0043(11) 0.0069(10) C52 0.0263(13) 0.0307(15) 0.0278(14) 0.0007(11) 0.0061(11) 0.0063(11) C53 0.0240(14) 0.0407(17) 0.0378(16) -0.0089(13) 0.0032(12) 0.0089(12) C54 0.0355(16) 0.0521(19) 0.0355(16) -0.0096(14) -0.0051(13) 0.0203(14) C55 0.0454(17) 0.0460(18) 0.0244(14) 0.0010(12) -0.0008(13) 0.0207(14) C56 0.0308(14) 0.0314(15) 0.0308(15) 0.0050(11) 0.0084(12) 0.0110(12) C57 0.0223(12) 0.0241(13) 0.0278(13) 0.0058(10) 0.0038(11) 0.0080(10) C58 0.0270(14) 0.0288(15) 0.0360(15) -0.0010(11) 0.0007(12) 0.0063(11) C59 0.0251(14) 0.0373(17) 0.056(2) 0.0031(14) 0.0029(14) -0.0008(13) C60 0.0237(14) 0.054(2) 0.0533(19) 0.0160(16) 0.0146(14) 0.0116(14) C61 0.0351(16) 0.0445(18) 0.0456(18) 0.0044(14) 0.0169(14) 0.0182(14) C62 0.0305(14) 0.0286(15) 0.0385(16) -0.0005(12) 0.0107(12) 0.0093(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O 1.8558(16) . ? Fe N1 2.083(2) . ? Fe N2 2.1096(19) . ? P1 N1 1.614(2) . ? P1 C1 1.739(3) . ? P1 C8 1.818(2) . ? P1 C2 1.820(2) . ? P2 N2 1.603(2) . ? P2 C1 1.737(2) . ? P2 C20 1.821(3) . ? P2 C14 1.833(2) . ? O C44 1.405(3) . ? N1 C26 1.420(3) . ? N2 C35 1.434(3) . ? C2 C7 1.394(4) . ? C2 C3 1.397(4) . ? C3 C4 1.398(4) . ? C4 C5 1.387(5) . ? C5 C6 1.381(5) . ? C6 C7 1.383(4) . ? C8 C13 1.384(4) . ? C8 C9 1.398(3) . ? C9 C10 1.384(4) . ? C10 C11 1.383(4) . ? C11 C12 1.384(4) . ? C12 C13 1.385(4) . ? C14 C19 1.380(4) . ? C14 C15 1.384(4) . ? C15 C16 1.388(4) . ? C16 C17 1.367(5) . ? C17 C18 1.375(5) . ? C18 C19 1.392(4) . ? C20 C21 1.394(4) . ? C20 C25 1.398(4) . ? C21 C22 1.390(4) . ? C22 C23 1.379(4) . ? C23 C24 1.365(5) . ? C24 C25 1.387(4) . ? C26 C31 1.413(3) . ? C26 C27 1.420(3) . ? C27 C28 1.385(3) . ? C27 C32 1.505(3) . ? C28 C29 1.380(4) . ? C29 C30 1.375(4) . ? C29 C33 1.512(4) . ? C30 C31 1.393(4) . ? C31 C34 1.509(4) . ? C35 C36 1.407(3) . ? C35 C40 1.412(3) . ? C36 C37 1.395(4) . ? C36 C41 1.504(4) . ? C37 C38 1.384(4) . ? C38 C39 1.382(4) . ? C38 C42 1.518(4) . ? C39 C40 1.395(4) . ? C40 C43 1.503(4) . ? C44 C51 1.538(3) . ? C44 C45 1.544(3) . ? C44 C57 1.545(3) . ? C45 C50 1.388(4) . ? C45 C46 1.390(4) . ? C46 C47 1.382(4) . ? C47 C48 1.377(4) . ? C48 C49 1.371(4) . ? C49 C50 1.397(4) . ? C51 C56 1.385(3) . ? C51 C52 1.402(3) . ? C52 C53 1.383(4) . ? C53 C54 1.374(4) . ? C54 C55 1.387(4) . ? C55 C56 1.389(4) . ? C57 C58 1.382(3) . ? C57 C62 1.392(3) . ? C58 C59 1.393(4) . ? C59 C60 1.374(4) . ? C60 C61 1.371(4) . ? C61 C62 1.389(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 O Fe N1 132.17(8) . . ? O Fe N2 123.32(8) . . ? N1 Fe N2 103.25(8) . . ? N1 P1 C1 106.77(11) . . ? N1 P1 C8 110.16(11) . . ? C1 P1 C8 115.82(11) . . ? N1 P1 C2 113.89(11) . . ? C1 P1 C2 101.77(12) . . ? C8 P1 C2 108.37(11) . . ? N2 P2 C1 103.90(11) . . ? N2 P2 C20 114.99(11) . . ? C1 P2 C20 105.88(12) . . ? N2 P2 C14 115.51(11) . . ? C1 P2 C14 113.77(12) . . ? C20 P2 C14 102.71(12) . . ? C44 O Fe 140.56(15) . . ? C26 N1 P1 132.70(17) . . ? C26 N1 Fe 129.99(15) . . ? P1 N1 Fe 95.48(9) . . ? C35 N2 P2 131.33(16) . . ? C35 N2 Fe 130.53(15) . . ? P2 N2 Fe 96.57(9) . . ? P2 C1 P1 128.23(15) . . ? P2 C1 Fe 83.99(9) . . ? P1 C1 Fe 82.49(10) . . ? C7 C2 C3 119.2(2) . . ? C7 C2 P1 121.8(2) . . ? C3 C2 P1 118.8(2) . . ? C2 C3 C4 120.7(3) . . ? C5 C4 C3 118.4(3) . . ? C6 C5 C4 121.6(3) . . ? C5 C6 C7 119.6(3) . . ? C6 C7 C2 120.4(3) . . ? C13 C8 C9 118.5(2) . . ? C13 C8 P1 117.43(19) . . ? C9 C8 P1 124.02(19) . . ? C10 C9 C8 120.3(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C12 119.7(3) . . ? C11 C12 C13 119.8(3) . . ? C8 C13 C12 121.2(3) . . ? C19 C14 C15 119.9(2) . . ? C19 C14 P2 122.0(2) . . ? C15 C14 P2 118.0(2) . . ? C14 C15 C16 119.9(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 120.0(3) . . ? C17 C18 C19 120.4(3) . . ? C14 C19 C18 119.5(3) . . ? C21 C20 C25 118.2(3) . . ? C21 C20 P2 119.08(19) . . ? C25 C20 P2 122.7(2) . . ? C22 C21 C20 120.9(3) . . ? C23 C22 C21 119.6(3) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 120.7(3) . . ? C24 C25 C20 120.2(3) . . ? C31 C26 N1 126.4(2) . . ? C31 C26 C27 117.3(2) . . ? N1 C26 C27 116.2(2) . . ? C28 C27 C26 120.2(2) . . ? C28 C27 C32 118.1(2) . . ? C26 C27 C32 121.7(2) . . ? C29 C28 C27 122.8(2) . . ? C30 C29 C28 116.9(2) . . ? C30 C29 C33 121.7(3) . . ? C28 C29 C33 121.5(3) . . ? C29 C30 C31 123.4(2) . . ? C30 C31 C26 119.4(2) . . ? C30 C31 C34 115.2(2) . . ? C26 C31 C34 125.3(2) . . ? C36 C35 C40 119.1(2) . . ? C36 C35 N2 120.4(2) . . ? C40 C35 N2 120.1(2) . . ? C37 C36 C35 118.9(2) . . ? C37 C36 C41 119.5(2) . . ? C35 C36 C41 121.7(2) . . ? C38 C37 C36 122.7(3) . . ? C39 C38 C37 117.6(2) . . ? C39 C38 C42 121.3(3) . . ? C37 C38 C42 121.1(3) . . ? C38 C39 C40 122.3(3) . . ? C39 C40 C35 119.3(2) . . ? C39 C40 C43 118.9(2) . . ? C35 C40 C43 121.8(2) . . ? O C44 C51 107.84(18) . . ? O C44 C45 110.61(19) . . ? C51 C44 C45 111.40(19) . . ? O C44 C57 108.86(19) . . ? C51 C44 C57 112.0(2) . . ? C45 C44 C57 106.10(19) . . ? C50 C45 C46 118.6(2) . . ? C50 C45 C44 123.2(2) . . ? C46 C45 C44 118.2(2) . . ? C47 C46 C45 120.6(3) . . ? C48 C47 C46 120.6(3) . . ? C49 C48 C47 119.5(3) . . ? C48 C49 C50 120.5(3) . . ? C45 C50 C49 120.2(3) . . ? C56 C51 C52 117.8(2) . . ? C56 C51 C44 124.7(2) . . ? C52 C51 C44 117.3(2) . . ? C53 C52 C51 121.3(3) . . ? C54 C53 C52 119.9(3) . . ? C53 C54 C55 119.9(3) . . ? C54 C55 C56 120.0(3) . . ? C51 C56 C55 121.1(3) . . ? C58 C57 C62 118.2(2) . . ? C58 C57 C44 120.2(2) . . ? C62 C57 C44 121.6(2) . . ? C57 C58 C59 120.7(3) . . ? C60 C59 C58 120.6(3) . . ? C61 C60 C59 119.3(3) . . ? C60 C61 C62 120.6(3) . . ? C61 C62 C57 120.7(3) . . ? #===END