# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 # start Validation Reply Form _vrf_PLAT773_FO3694 ; PROBLEM: Suspect C-C Bond in CIF: C3TA -- C4TA .. 1.71 Ang. RESPONSE: The thf-molecule is disordered. ; _vrf_PLAT761_FO3694 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO3694 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE:All hydrogen positions were calculated. ; _vrf_PLAT761_FO3617 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE:All hydrogen positions were calculated. ; _vrf_PLAT762_FO3617 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE:All hydrogen positions were calculated. ; # end Validation Reply Form #Added by publCIF (CCDC output) (Di 16. Jun 09:57:07 2009) _audit_update_record ; 2009-06-16 # Formatted by publCIF ; # 1. SUBMISSION DETAILS _publ_contact_author ; Matthias Westerhausen Institut f\"ur Anorganische und Analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 07743 Jena Germany ; _publ_contact_author_phone '03641 948 110' _publ_contact_author_fax '03641 948 102' _publ_contact_author_email m.we@uni-jena.de # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Heteroleptic Iron(II) 2-Pyridylmethylamides and 2-Pyridylmethylideneamines via the Reaction of (thf)Fe[N(SiMe~3~)~2~]~2~Cl with (2-Pyridylmethyl) (trialkylsilyl)amines ; loop_ _publ_author_name _publ_author_address 'Matthias Westerhausen' ; Institut f\"ur Anorganische und Analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Astrid Malassa' ; Institut f\"ur Anorganische und Analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'ANicole Herzer' ; Institut f\"ur Anorganische und Analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; H.Gorls ; Institut f\"ur Anorganische und Analytische Chemie Friedrich-Schiller-Universit\"at Jena Lessing-Str. 8 D-07743 Jena Germany ; _publ_contact_author_name 'Matthias Westerhausen' # data_FO3159 _database_code_depnum_ccdc_archive 'CCDC 676619' _audit_update_record ; 2008-02-01 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 N2 Si' _chemical_formula_weight 366.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 6.4898(3) _cell_length_b 10.3387(6) _cell_length_c 15.1982(8) _cell_angle_alpha 93.801(2) _cell_angle_beta 100.954(3) _cell_angle_gamma 99.192(3) _cell_volume 983.38(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 6965 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6965 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4448 _reflns_number_gt 2950 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECET _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0529P)^2^+0.1600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4448 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.53117(8) 0.20884(6) 0.25044(4) 0.02180(16) Uani 1 1 d . . . N1 N 0.7605(3) 0.32409(18) 0.27483(13) 0.0281(4) Uani 1 1 d . . . N2 N 1.0901(3) 0.61547(18) 0.39708(12) 0.0305(4) Uani 1 1 d . . . C1 C 0.7861(3) 0.4515(2) 0.32676(16) 0.0342(6) Uani 1 1 d . . . H1A H 0.7865 0.4377 0.3906 0.041 Uiso 1 1 calc R . . H1B H 0.6631 0.4943 0.3042 0.041 Uiso 1 1 calc R . . C2 C 0.9894(3) 0.5413(2) 0.32090(14) 0.0253(5) Uani 1 1 d . . . C3 C 1.0665(3) 0.5460(2) 0.24212(15) 0.0303(5) Uani 1 1 d . . . H3A H 0.9908 0.4925 0.1890 0.036 Uiso 1 1 calc R . . C4 C 1.2551(3) 0.6294(2) 0.24174(16) 0.0336(5) Uani 1 1 d . . . H4A H 1.3104 0.6343 0.1883 0.040 Uiso 1 1 calc R . . C5 C 1.3619(3) 0.7055(2) 0.31974(16) 0.0336(5) Uani 1 1 d . . . H5A H 1.4924 0.7633 0.3215 0.040 Uiso 1 1 calc R . . C6 C 1.2737(3) 0.6952(2) 0.39533(16) 0.0335(5) Uani 1 1 d . . . H6A H 1.3472 0.7477 0.4492 0.040 Uiso 1 1 calc R . . C7 C 0.3917(3) 0.1933(2) 0.34812(13) 0.0219(4) Uani 1 1 d . . . C8 C 0.3619(3) 0.0785(2) 0.39039(14) 0.0256(5) Uani 1 1 d . . . H8A H 0.4129 0.0034 0.3694 0.031 Uiso 1 1 calc R . . C9 C 0.2589(3) 0.0715(2) 0.46278(14) 0.0288(5) Uani 1 1 d . . . H9A H 0.2406 -0.0078 0.4909 0.035 Uiso 1 1 calc R . . C10 C 0.1830(3) 0.1798(2) 0.49385(14) 0.0296(5) Uani 1 1 d . . . H10A H 0.1132 0.1752 0.5434 0.036 Uiso 1 1 calc R . . C11 C 0.2091(3) 0.2948(2) 0.45263(14) 0.0310(5) Uani 1 1 d . . . H11A H 0.1562 0.3691 0.4735 0.037 Uiso 1 1 calc R . . C12 C 0.3127(3) 0.3015(2) 0.38066(14) 0.0266(5) Uani 1 1 d . . . H12A H 0.3304 0.3811 0.3529 0.032 Uiso 1 1 calc R . . C13 C 0.6147(3) 0.0506(2) 0.21815(13) 0.0227(4) Uani 1 1 d . . . C14 C 0.5243(4) -0.0252(2) 0.13603(15) 0.0340(5) Uani 1 1 d . . . H14A H 0.4118 0.0021 0.0961 0.041 Uiso 1 1 calc R . . C15 C 0.5955(4) -0.1393(3) 0.11184(17) 0.0429(6) Uani 1 1 d . . . H15A H 0.5317 -0.1891 0.0558 0.051 Uiso 1 1 calc R . . C16 C 0.7593(4) -0.1808(2) 0.16910(16) 0.0383(6) Uani 1 1 d . . . H16A H 0.8080 -0.2590 0.1525 0.046 Uiso 1 1 calc R . . C17 C 0.8519(3) -0.1075(2) 0.25076(15) 0.0314(5) Uani 1 1 d . . . H17A H 0.9647 -0.1354 0.2903 0.038 Uiso 1 1 calc R . . C18 C 0.7801(3) 0.0059(2) 0.27463(14) 0.0262(5) Uani 1 1 d . . . H18A H 0.8446 0.0551 0.3309 0.031 Uiso 1 1 calc R . . C19 C 0.3388(3) 0.2578(2) 0.15590(13) 0.0236(5) Uani 1 1 d . . . C20 C 0.3980(4) 0.3597(2) 0.10514(15) 0.0311(5) Uani 1 1 d . . . H20A H 0.5409 0.4057 0.1183 0.037 Uiso 1 1 calc R . . C21 C 0.2521(4) 0.3953(3) 0.03564(16) 0.0391(6) Uani 1 1 d . . . H21A H 0.2953 0.4659 0.0024 0.047 Uiso 1 1 calc R . . C22 C 0.0453(4) 0.3285(3) 0.01488(16) 0.0415(6) Uani 1 1 d . . . H22A H -0.0540 0.3524 -0.0330 0.050 Uiso 1 1 calc R . . C23 C -0.0179(4) 0.2266(3) 0.06361(16) 0.0412(6) Uani 1 1 d . . . H23A H -0.1605 0.1801 0.0491 0.049 Uiso 1 1 calc R . . C24 C 0.1270(3) 0.1924(2) 0.13369(15) 0.0327(5) Uani 1 1 d . . . H24A H 0.0815 0.1229 0.1674 0.039 Uiso 1 1 calc R . . H1N1 H 0.874(4) 0.294(2) 0.2839(17) 0.040(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0207(3) 0.0215(3) 0.0229(3) 0.0014(2) 0.0046(2) 0.0029(2) N1 0.0207(9) 0.0253(10) 0.0373(11) -0.0039(8) 0.0071(8) 0.0030(7) N2 0.0288(9) 0.0267(11) 0.0343(11) -0.0037(8) 0.0074(8) 0.0019(8) C1 0.0277(11) 0.0310(13) 0.0422(14) -0.0101(11) 0.0129(11) -0.0013(9) C2 0.0238(10) 0.0208(11) 0.0315(12) -0.0002(9) 0.0053(9) 0.0064(8) C3 0.0306(11) 0.0297(13) 0.0285(12) -0.0006(10) 0.0039(10) 0.0025(9) C4 0.0364(12) 0.0299(13) 0.0365(13) 0.0063(10) 0.0125(11) 0.0040(10) C5 0.0270(11) 0.0269(13) 0.0453(14) 0.0017(11) 0.0084(10) -0.0002(9) C6 0.0281(11) 0.0281(13) 0.0391(13) -0.0067(10) 0.0029(10) -0.0017(9) C7 0.0180(9) 0.0251(11) 0.0200(10) 0.0018(9) -0.0004(8) 0.0015(8) C8 0.0225(10) 0.0268(12) 0.0256(11) 0.0004(9) 0.0011(9) 0.0037(8) C9 0.0241(10) 0.0331(13) 0.0273(12) 0.0089(10) 0.0023(9) 0.0006(9) C10 0.0233(10) 0.0430(15) 0.0229(11) 0.0044(10) 0.0057(9) 0.0048(10) C11 0.0311(11) 0.0348(14) 0.0288(12) -0.0015(10) 0.0082(10) 0.0099(10) C12 0.0263(10) 0.0286(12) 0.0262(11) 0.0046(9) 0.0052(9) 0.0081(9) C13 0.0221(10) 0.0246(11) 0.0215(10) 0.0014(9) 0.0066(8) 0.0019(8) C14 0.0373(12) 0.0328(14) 0.0305(12) -0.0024(10) -0.0008(10) 0.0135(10) C15 0.0546(15) 0.0406(15) 0.0308(13) -0.0113(11) -0.0017(11) 0.0193(12) C16 0.0492(14) 0.0329(14) 0.0380(14) 0.0001(11) 0.0129(12) 0.0191(11) C17 0.0284(11) 0.0361(14) 0.0333(13) 0.0093(11) 0.0084(10) 0.0118(10) C18 0.0271(11) 0.0278(12) 0.0237(11) 0.0024(9) 0.0048(9) 0.0054(9) C19 0.0265(10) 0.0257(12) 0.0216(10) 0.0014(9) 0.0086(8) 0.0094(9) C20 0.0381(12) 0.0285(13) 0.0297(12) 0.0059(10) 0.0125(10) 0.0071(10) C21 0.0552(16) 0.0396(15) 0.0304(13) 0.0136(11) 0.0160(12) 0.0192(12) C22 0.0465(15) 0.0572(18) 0.0262(12) 0.0090(12) 0.0026(11) 0.0287(13) C23 0.0288(12) 0.0570(18) 0.0373(14) 0.0059(12) 0.0014(10) 0.0114(11) C24 0.0272(11) 0.0388(14) 0.0332(13) 0.0091(11) 0.0072(10) 0.0058(10) _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 Si N1 1.7141(18) . ? Si C13 1.868(2) . ? Si C19 1.870(2) . ? Si C7 1.8827(19) . ? N1 C1 1.459(3) . ? N1 H1N1 0.84(2) . ? N2 C2 1.338(3) . ? N2 C6 1.342(3) . ? C1 C2 1.509(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.383(3) . ? C3 C4 1.381(3) . ? C3 H3A 0.9500 . ? C4 C5 1.376(3) . ? C4 H4A 0.9500 . ? C5 C6 1.380(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.391(3) . ? C7 C12 1.402(3) . ? C8 C9 1.392(3) . ? C8 H8A 0.9500 . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 C11 1.381(3) . ? C10 H10A 0.9500 . ? C11 C12 1.389(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.401(3) . ? C13 C14 1.400(3) . ? C14 C15 1.386(3) . ? C14 H14A 0.9500 . ? C15 C16 1.384(3) . ? C15 H15A 0.9500 . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.381(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.394(3) . ? C19 C24 1.399(3) . ? C20 C21 1.389(3) . ? C20 H20A 0.9500 . ? C21 C22 1.376(4) . ? C21 H21A 0.9500 . ? C22 C23 1.381(4) . ? C22 H22A 0.9500 . ? C23 C24 1.385(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? 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 Si C13 105.56(9) . . ? N1 Si C19 109.59(10) . . ? C13 Si C19 111.47(9) . . ? N1 Si C7 112.74(9) . . ? C13 Si C7 111.02(9) . . ? C19 Si C7 106.56(8) . . ? C1 N1 Si 125.01(14) . . ? C1 N1 H1N1 111.1(17) . . ? Si N1 H1N1 115.4(17) . . ? C2 N2 C6 117.44(18) . . ? N1 C1 C2 112.28(16) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C3 122.44(19) . . ? N2 C2 C1 115.43(18) . . ? C3 C2 C1 122.12(19) . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C5 C4 C3 119.2(2) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 118.0(2) . . ? C4 C5 H5A 121.0 . . ? C6 C5 H5A 121.0 . . ? N2 C6 C5 123.8(2) . . ? N2 C6 H6A 118.1 . . ? C5 C6 H6A 118.1 . . ? C8 C7 C12 117.55(18) . . ? C8 C7 Si 123.13(15) . . ? C12 C7 Si 119.32(16) . . ? C7 C8 C9 121.3(2) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C10 C9 C8 120.0(2) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 119.84(19) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 119.9(2) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C7 121.4(2) . . ? C11 C12 H12A 119.3 . . ? C7 C12 H12A 119.3 . . ? C18 C13 C14 117.02(19) . . ? C18 C13 Si 120.45(15) . . ? C14 C13 Si 122.47(16) . . ? C15 C14 C13 121.4(2) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 119.6(2) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C13 121.8(2) . . ? C17 C18 H18A 119.1 . . ? C13 C18 H18A 119.1 . . ? C20 C19 C24 117.3(2) . . ? C20 C19 Si 122.22(16) . . ? C24 C19 Si 120.44(16) . . ? C21 C20 C19 121.3(2) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C22 C21 C20 120.0(2) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 119.9(2) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C19 121.4(2) . . ? C23 C24 H24A 119.3 . . ? C19 C24 H24A 119.3 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.277 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.056 #=== END data_FO2925 _database_code_depnum_ccdc_archive 'CCDC 676620' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 Cl2 Fe2 N4 Si2' _chemical_formula_weight 711.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4163(7) _cell_length_b 10.9918(13) _cell_length_c 11.0332(12) _cell_angle_alpha 112.081(5) _cell_angle_beta 99.969(6) _cell_angle_gamma 94.411(6) _cell_volume 920.20(17) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 6066 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 27.41 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6066 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.41 _reflns_number_total 4028 _reflns_number_gt 2902 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0422P)^2^+0.1861P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4028 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 1.09609(4) 0.50215(4) 0.11416(4) 0.02507(13) Uani 1 1 d . . . Cl Cl 1.33346(8) 0.59431(8) 0.26584(8) 0.0429(2) Uani 1 1 d . . . Si Si 0.93057(8) 0.76632(7) 0.15325(7) 0.02482(18) Uani 1 1 d . . . N1 N 0.9547(3) 0.4364(2) 0.2216(2) 0.0277(5) Uani 1 1 d . . . N2 N 0.8901(2) 0.5921(2) 0.0789(2) 0.0231(5) Uani 1 1 d . . . C1 C 1.0058(4) 0.3778(3) 0.3064(3) 0.0342(7) Uani 1 1 d . . . H1A H 1.1132 0.3562 0.3133 0.041 Uiso 1 1 calc R . . C2 C 0.9090(4) 0.3485(3) 0.3828(3) 0.0400(7) Uani 1 1 d . . . H2A H 0.9484 0.3075 0.4416 0.048 Uiso 1 1 calc R . . C3 C 0.7522(4) 0.3801(3) 0.3722(3) 0.0417(8) Uani 1 1 d . . . H3A H 0.6828 0.3622 0.4248 0.050 Uiso 1 1 calc R . . C4 C 0.6983(3) 0.4377(3) 0.2845(3) 0.0345(7) Uani 1 1 d . . . H4A H 0.5902 0.4579 0.2745 0.041 Uiso 1 1 calc R . . C5 C 0.8031(3) 0.4662(3) 0.2108(3) 0.0258(6) Uani 1 1 d . . . C6 C 0.7507(3) 0.5297(3) 0.1137(3) 0.0291(6) Uani 1 1 d . . . C7 C 0.9526(4) 0.8199(3) 0.3383(3) 0.0410(7) Uani 1 1 d . . . H7A H 1.0368 0.7768 0.3723 0.062 Uiso 1 1 calc R . . H7B H 0.8484 0.7945 0.3571 0.062 Uiso 1 1 calc R . . H7C H 0.9843 0.9167 0.3825 0.062 Uiso 1 1 calc R . . C8 C 1.1278(3) 0.8201(3) 0.1199(3) 0.0357(7) Uani 1 1 d . . . H8A H 1.2135 0.7779 0.1533 0.054 Uiso 1 1 calc R . . H8B H 1.1568 0.9169 0.1656 0.054 Uiso 1 1 calc R . . H8C H 1.1168 0.7939 0.0232 0.054 Uiso 1 1 calc R . . C9 C 0.7668(3) 0.8504(3) 0.0869(3) 0.0293(6) Uani 1 1 d . . . C10 C 0.5932(3) 0.7966(3) 0.0873(3) 0.0420(8) Uani 1 1 d . . . H10A H 0.5149 0.8434 0.0523 0.063 Uiso 1 1 calc R . . H10B H 0.5856 0.8108 0.1791 0.063 Uiso 1 1 calc R . . H10C H 0.5682 0.7013 0.0306 0.063 Uiso 1 1 calc R . . C11 C 0.8019(4) 1.0004(3) 0.1743(3) 0.0481(8) Uani 1 1 d . . . H11A H 0.7182 1.0444 0.1411 0.072 Uiso 1 1 calc R . . H11B H 0.9096 1.0375 0.1703 0.072 Uiso 1 1 calc R . . H11C H 0.8001 1.0149 0.2673 0.072 Uiso 1 1 calc R . . C12 C 0.7701(4) 0.8292(3) -0.0583(3) 0.0436(8) Uani 1 1 d . . . H12A H 0.6856 0.8726 -0.0914 0.065 Uiso 1 1 calc R . . H12B H 0.7493 0.7338 -0.1146 0.065 Uiso 1 1 calc R . . H12C H 0.8774 0.8677 -0.0616 0.065 Uiso 1 1 calc R . . C1H C 0.5613(3) 0.9534(3) 0.5024(3) 0.0384(7) Uani 1 1 d . . . H1HA H 0.5546 0.8878 0.4103 0.046 Uiso 1 1 calc R . . H1HB H 0.6726 1.0055 0.5357 0.046 Uiso 1 1 calc R . . C2H C 0.5356(4) 0.8798(3) 0.5905(3) 0.0395(7) Uani 1 1 d . . . H2HA H 0.4227 0.8310 0.5602 0.047 Uiso 1 1 calc R . . H2HB H 0.5483 0.9449 0.6838 0.047 Uiso 1 1 calc R . . C3H C 0.6554(4) 0.7814(3) 0.5879(3) 0.0487(8) Uani 1 1 d . . . H3HA H 0.6342 0.7368 0.6468 0.073 Uiso 1 1 calc R . . H3HB H 0.7675 0.8293 0.6192 0.073 Uiso 1 1 calc R . . H3HC H 0.6413 0.7151 0.4962 0.073 Uiso 1 1 calc R . . H6A H 0.678(3) 0.597(3) 0.153(3) 0.030(7) Uiso 1 1 d . . . H6B H 0.681(3) 0.462(3) 0.038(3) 0.029(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0232(2) 0.0272(2) 0.0244(2) 0.00984(17) 0.00438(16) 0.00512(16) Cl 0.0311(4) 0.0483(5) 0.0403(4) 0.0134(4) -0.0045(3) 0.0039(3) Si 0.0259(4) 0.0221(4) 0.0258(4) 0.0079(3) 0.0077(3) 0.0031(3) N1 0.0324(12) 0.0259(12) 0.0254(12) 0.0097(10) 0.0083(10) 0.0066(10) N2 0.0185(10) 0.0236(12) 0.0290(12) 0.0113(10) 0.0073(9) 0.0035(9) C1 0.0419(17) 0.0315(16) 0.0332(16) 0.0154(13) 0.0095(14) 0.0124(14) C2 0.059(2) 0.0353(17) 0.0335(17) 0.0199(14) 0.0125(15) 0.0130(15) C3 0.0490(18) 0.0426(19) 0.0447(19) 0.0253(16) 0.0212(16) 0.0048(15) C4 0.0337(15) 0.0313(16) 0.0417(18) 0.0158(14) 0.0138(14) 0.0028(13) C5 0.0306(14) 0.0187(14) 0.0251(14) 0.0055(11) 0.0066(12) 0.0007(11) C6 0.0255(14) 0.0316(16) 0.0337(17) 0.0164(14) 0.0072(13) 0.0043(13) C7 0.0499(19) 0.0379(18) 0.0293(16) 0.0086(14) 0.0060(14) 0.0032(15) C8 0.0328(15) 0.0307(16) 0.0436(18) 0.0143(14) 0.0110(14) 0.0013(13) C9 0.0307(14) 0.0247(15) 0.0339(16) 0.0108(12) 0.0110(13) 0.0075(12) C10 0.0325(16) 0.045(2) 0.055(2) 0.0267(17) 0.0105(15) 0.0116(14) C11 0.0517(19) 0.0315(18) 0.060(2) 0.0156(16) 0.0118(17) 0.0132(15) C12 0.0528(19) 0.051(2) 0.0414(19) 0.0293(16) 0.0150(16) 0.0212(16) C1H 0.0381(16) 0.0397(18) 0.0396(18) 0.0173(15) 0.0106(14) 0.0059(14) C2H 0.0433(17) 0.0394(18) 0.0373(18) 0.0173(15) 0.0078(14) 0.0063(14) C3H 0.054(2) 0.049(2) 0.048(2) 0.0243(17) 0.0086(17) 0.0162(17) _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 N2 2.018(2) 2_765 ? Fe N1 2.084(2) . ? Fe N2 2.1107(19) . ? Fe Cl 2.2527(8) . ? Fe Fe 2.7298(8) 2_765 ? Si N2 1.754(2) . ? Si C8 1.861(3) . ? Si C7 1.870(3) . ? Si C9 1.909(3) . ? N1 C5 1.339(3) . ? N1 C1 1.353(3) . ? N2 C6 1.490(3) . ? N2 Fe 2.018(2) 2_765 ? C1 C2 1.371(4) . ? C2 C3 1.386(4) . ? C3 C4 1.377(4) . ? C4 C5 1.391(4) . ? C5 C6 1.509(4) . ? C9 C10 1.535(4) . ? C9 C12 1.535(4) . ? C9 C11 1.539(4) . ? C1H C2H 1.511(4) . ? C1H C1H 1.517(5) 2_676 ? C2H C3H 1.530(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 N2 Fe N1 127.91(9) 2_765 . ? N2 Fe N2 97.24(7) 2_765 . ? N1 Fe N2 82.01(8) . . ? N2 Fe Cl 117.03(6) 2_765 . ? N1 Fe Cl 102.09(7) . . ? N2 Fe Cl 128.61(6) . . ? N2 Fe Fe 50.09(6) 2_765 2_765 ? N1 Fe Fe 110.28(6) . 2_765 ? N2 Fe Fe 47.15(6) . 2_765 ? Cl Fe Fe 144.93(3) . 2_765 ? N2 Si C8 107.93(11) . . ? N2 Si C7 108.21(13) . . ? C8 Si C7 108.86(14) . . ? N2 Si C9 113.94(12) . . ? C8 Si C9 108.26(12) . . ? C7 Si C9 109.52(13) . . ? C5 N1 C1 118.8(2) . . ? C5 N1 Fe 114.53(17) . . ? C1 N1 Fe 126.42(18) . . ? C6 N2 Si 115.56(17) . . ? C6 N2 Fe 112.90(17) . 2_765 ? Si N2 Fe 119.06(11) . 2_765 ? C6 N2 Fe 108.50(15) . . ? Si N2 Fe 113.17(11) . . ? Fe N2 Fe 82.76(7) 2_765 . ? N1 C1 C2 122.8(3) . . ? C1 C2 C3 118.4(3) . . ? C4 C3 C2 119.3(3) . . ? C3 C4 C5 119.5(3) . . ? N1 C5 C4 121.2(2) . . ? N1 C5 C6 117.0(2) . . ? C4 C5 C6 121.8(2) . . ? N2 C6 C5 113.5(2) . . ? C10 C9 C12 107.1(2) . . ? C10 C9 C11 108.5(2) . . ? C12 C9 C11 108.9(2) . . ? C10 C9 Si 113.26(19) . . ? C12 C9 Si 110.10(18) . . ? C11 C9 Si 108.9(2) . . ? C2H C1H C1H 113.8(3) . 2_676 ? C1H C2H C3H 112.7(2) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.334 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.072 #=== END data_FO2947 _database_code_depnum_ccdc_archive 'CCDC 676621' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H50 Cl2 Fe2 N4 Si2' _chemical_formula_weight 681.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3393(5) _cell_length_b 11.7681(3) _cell_length_c 14.5255(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.333(2) _cell_angle_gamma 90.00 _cell_volume 1743.98(13) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12182 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12182 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3986 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXTL/PC _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^)+(0.0518P)^2^+0.2553P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3986 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.51261(3) 0.43039(2) -0.07414(2) 0.02483(11) Uani 1 1 d . . . Cl Cl 0.61142(7) 0.40617(5) -0.20079(4) 0.03669(16) Uani 1 1 d . . . Si Si 0.74741(6) 0.40495(5) 0.09997(4) 0.02831(16) Uani 1 1 d . . . N1 N 0.44180(18) 0.26783(14) -0.05540(12) 0.0262(4) Uani 1 1 d . . . N2 N 0.57595(18) 0.41697(13) 0.07111(12) 0.0244(4) Uani 1 1 d . . . C1 C 0.3980(2) 0.19106(17) -0.12218(15) 0.0298(5) Uani 1 1 d . . . H1A H 0.3990 0.2107 -0.1855 0.036 Uiso 1 1 calc R . . C2 C 0.3523(2) 0.08631(18) -0.10273(17) 0.0332(5) Uani 1 1 d . . . H2A H 0.3224 0.0341 -0.1514 0.040 Uiso 1 1 calc R . . C3 C 0.3506(3) 0.05813(19) -0.01056(17) 0.0371(6) Uani 1 1 d . . . H3A H 0.3179 -0.0136 0.0049 0.045 Uiso 1 1 calc R . . C4 C 0.3967(2) 0.13516(18) 0.05889(16) 0.0320(5) Uani 1 1 d . . . H4A H 0.3966 0.1167 0.1225 0.038 Uiso 1 1 calc R . . C5 C 0.4433(2) 0.23961(16) 0.03459(15) 0.0246(4) Uani 1 1 d . . . C6 C 0.4975(2) 0.32616(17) 0.10706(14) 0.0268(5) Uani 1 1 d . . . H6A H 0.4238 0.3617 0.1322 0.032 Uiso 1 1 calc R . . H6B H 0.5533 0.2867 0.1592 0.032 Uiso 1 1 calc R . . C7 C 0.8150(2) 0.5093(2) 0.02293(17) 0.0410(6) Uani 1 1 d . . . H7A H 0.7813 0.4917 -0.0425 0.062 Uiso 1 1 calc R . . H7B H 0.9109 0.5045 0.0337 0.062 Uiso 1 1 calc R . . H7C H 0.7881 0.5863 0.0373 0.062 Uiso 1 1 calc R . . C8 C 0.7885(3) 0.2547(2) 0.0710(2) 0.0485(7) Uani 1 1 d . . . H8A H 0.7549 0.2393 0.0052 0.073 Uiso 1 1 calc R . . H8B H 0.7483 0.2019 0.1102 0.073 Uiso 1 1 calc R . . H8C H 0.8839 0.2445 0.0826 0.073 Uiso 1 1 calc R . . C9 C 0.8132(2) 0.43787(17) 0.22869(16) 0.0301(5) Uani 1 1 d . . . C10 C 0.8337(3) 0.56751(19) 0.24050(19) 0.0454(7) Uani 1 1 d . . . H10A H 0.8667 0.5849 0.3061 0.068 Uiso 1 1 calc R . . H10B H 0.7500 0.6066 0.2212 0.068 Uiso 1 1 calc R . . H10C H 0.8972 0.5932 0.2017 0.068 Uiso 1 1 calc R . . C11 C 0.7102(2) 0.40377(19) 0.28913(16) 0.0340(5) Uani 1 1 d . . . H11A H 0.7437 0.4207 0.3547 0.051 Uiso 1 1 calc R . . H11B H 0.6921 0.3222 0.2820 0.051 Uiso 1 1 calc R . . H11C H 0.6293 0.4467 0.2692 0.051 Uiso 1 1 calc R . . C12 C 0.9424(2) 0.3706(2) 0.26299(18) 0.0419(6) Uani 1 1 d . . . H12A H 0.9212 0.2882 0.2525 0.050 Uiso 1 1 calc R . . C13 C 1.0541(3) 0.3976(3) 0.2087(2) 0.0546(8) Uani 1 1 d . . . H13A H 1.1310 0.3516 0.2332 0.082 Uiso 1 1 calc R . . H13B H 1.0766 0.4784 0.2158 0.082 Uiso 1 1 calc R . . H13C H 1.0260 0.3802 0.1425 0.082 Uiso 1 1 calc R . . C14 C 0.9945(3) 0.3847(3) 0.3680(2) 0.0692(10) Uani 1 1 d . . . H14A H 0.9246 0.3669 0.4039 0.104 Uiso 1 1 calc R . . H14B H 1.0236 0.4633 0.3806 0.104 Uiso 1 1 calc R . . H14C H 1.0685 0.3330 0.3863 0.104 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 0.0345(2) 0.02442(17) 0.01611(17) 0.00015(11) 0.00557(13) -0.00123(12) Cl 0.0537(4) 0.0363(3) 0.0233(3) -0.0006(2) 0.0160(3) 0.0011(2) Si 0.0306(4) 0.0334(3) 0.0211(3) -0.0011(2) 0.0046(3) 0.0007(2) N1 0.0326(11) 0.0277(9) 0.0183(9) -0.0004(7) 0.0043(8) -0.0006(7) N2 0.0301(10) 0.0254(9) 0.0176(9) 0.0001(7) 0.0034(8) -0.0032(7) C1 0.0361(14) 0.0327(11) 0.0198(11) -0.0032(9) 0.0024(10) 0.0006(9) C2 0.0396(14) 0.0325(12) 0.0264(12) -0.0065(9) 0.0024(11) -0.0040(10) C3 0.0509(16) 0.0292(12) 0.0306(13) -0.0002(10) 0.0051(12) -0.0107(10) C4 0.0432(15) 0.0313(11) 0.0215(11) 0.0028(9) 0.0053(10) -0.0054(10) C5 0.0257(12) 0.0262(10) 0.0219(11) 0.0013(8) 0.0040(9) 0.0007(8) C6 0.0346(13) 0.0273(10) 0.0188(10) 0.0017(8) 0.0051(9) -0.0046(9) C7 0.0332(14) 0.0619(16) 0.0284(13) 0.0063(11) 0.0063(11) -0.0078(12) C8 0.0490(17) 0.0489(15) 0.0465(16) -0.0149(12) 0.0040(13) 0.0121(12) C9 0.0316(13) 0.0325(12) 0.0249(12) 0.0021(9) 0.0007(10) -0.0037(9) C10 0.0583(18) 0.0410(14) 0.0349(15) -0.0029(11) 0.0014(13) -0.0130(12) C11 0.0381(14) 0.0420(13) 0.0212(12) -0.0036(9) 0.0021(10) -0.0028(10) C12 0.0339(14) 0.0566(15) 0.0339(14) 0.0074(12) 0.0014(11) 0.0023(12) C13 0.0365(16) 0.082(2) 0.0444(18) 0.0081(15) 0.0040(14) 0.0022(14) C14 0.0456(19) 0.119(3) 0.0390(18) 0.0224(18) -0.0054(15) 0.0055(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N2 2.0200(17) 3_665 ? Fe N1 2.0820(17) . ? Fe N2 2.1111(18) . ? Fe Cl 2.2625(6) . ? Fe Fe 2.7520(6) 3_665 ? Si N2 1.760(2) . ? Si C7 1.871(2) . ? Si C8 1.882(2) . ? Si C9 1.923(2) . ? N1 C5 1.346(3) . ? N1 C1 1.349(3) . ? N2 C6 1.487(2) . ? N2 Fe 2.0199(17) 3_665 ? C1 C2 1.366(3) . ? C2 C3 1.382(3) . ? C3 C4 1.382(3) . ? C4 C5 1.387(3) . ? C5 C6 1.506(3) . ? C9 C11 1.539(3) . ? C9 C10 1.546(3) . ? C9 C12 1.563(3) . ? C12 C13 1.533(4) . ? C12 C14 1.542(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 N2 Fe N1 130.09(7) 3_665 . ? N2 Fe N2 96.49(7) 3_665 . ? N1 Fe N2 81.91(7) . . ? N2 Fe Cl 113.32(5) 3_665 . ? N1 Fe Cl 101.84(5) . . ? N2 Fe Cl 134.06(5) . . ? N2 Fe Fe 49.66(5) 3_665 3_665 ? N1 Fe Fe 111.39(5) . 3_665 ? N2 Fe Fe 46.83(5) . 3_665 ? Cl Fe Fe 145.49(2) . 3_665 ? N2 Si C7 105.32(10) . . ? N2 Si C8 106.12(11) . . ? C7 Si C8 111.29(12) . . ? N2 Si C9 113.54(10) . . ? C7 Si C9 109.99(11) . . ? C8 Si C9 110.44(11) . . ? C5 N1 C1 118.86(18) . . ? C5 N1 Fe 113.87(13) . . ? C1 N1 Fe 127.26(14) . . ? C6 N2 Si 116.39(14) . . ? C6 N2 Fe 110.89(13) . 3_665 ? Si N2 Fe 120.59(9) . 3_665 ? C6 N2 Fe 107.84(13) . . ? Si N2 Fe 112.41(9) . . ? Fe N2 Fe 83.51(7) 3_665 . ? N1 C1 C2 122.9(2) . . ? C1 C2 C3 118.4(2) . . ? C4 C3 C2 119.5(2) . . ? C3 C4 C5 119.3(2) . . ? N1 C5 C4 121.07(19) . . ? N1 C5 C6 117.15(17) . . ? C4 C5 C6 121.79(19) . . ? N2 C6 C5 113.76(17) . . ? C11 C9 C10 106.8(2) . . ? C11 C9 C12 108.71(18) . . ? C10 C9 C12 111.7(2) . . ? C11 C9 Si 109.49(16) . . ? C10 C9 Si 109.10(16) . . ? C12 C9 Si 110.94(16) . . ? C13 C12 C14 108.3(2) . . ? C13 C12 C9 114.0(2) . . ? C14 C12 C9 113.8(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.296 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.069 #=== END data_FO2942 _database_code_depnum_ccdc_archive 'CCDC 676622' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 Cl2 Fe2 N4 Si2' _chemical_formula_weight 709.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6409(4) _cell_length_b 11.7277(7) _cell_length_c 17.5459(9) _cell_angle_alpha 73.229(3) _cell_angle_beta 88.473(3) _cell_angle_gamma 70.858(3) _cell_volume 1789.36(16) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12389 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.052 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12389 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8068 _reflns_number_gt 5781 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0460P)^2^+1.3992P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8068 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.10117(4) 0.77540(4) 0.73688(2) 0.02248(11) Uani 1 1 d . . . Fe2 Fe 0.85678(4) 0.70081(4) 0.74745(2) 0.02264(11) Uani 1 1 d . . . Cl1 Cl 1.20564(8) 0.90976(7) 0.65951(5) 0.03638(19) Uani 1 1 d . . . Cl2 Cl 0.72919(8) 0.57970(8) 0.81753(5) 0.03725(19) Uani 1 1 d . . . Si1 Si 0.81464(8) 0.96301(7) 0.80410(5) 0.02629(18) Uani 1 1 d . . . Si2 Si 1.16419(8) 0.49716(7) 0.70820(5) 0.02516(18) Uani 1 1 d . . . N1 N 0.7547(2) 0.7568(2) 0.63352(13) 0.0258(5) Uani 1 1 d . . . N2 N 1.0484(2) 0.6563(2) 0.68639(13) 0.0233(5) Uani 1 1 d . . . N3 N 1.2133(2) 0.7189(2) 0.84911(13) 0.0237(5) Uani 1 1 d . . . N4 N 0.9174(2) 0.8063(2) 0.80578(13) 0.0223(5) Uani 1 1 d . . . C1 C 0.6086(3) 0.7920(3) 0.61406(18) 0.0302(6) Uani 1 1 d . . . H1A H 0.5440 0.7849 0.6557 0.036 Uiso 1 1 calc R . . C2 C 0.5510(3) 0.8373(3) 0.53670(19) 0.0350(7) Uani 1 1 d . . . H2A H 0.4483 0.8598 0.5247 0.042 Uiso 1 1 calc R . . C3 C 0.6444(3) 0.8499(3) 0.47615(19) 0.0386(8) Uani 1 1 d . . . H3A H 0.6061 0.8837 0.4220 0.046 Uiso 1 1 calc R . . C4 C 0.7937(3) 0.8129(3) 0.49508(17) 0.0316(7) Uani 1 1 d . . . H4A H 0.8597 0.8203 0.4542 0.038 Uiso 1 1 calc R . . C5 C 0.8459(3) 0.7649(3) 0.57474(16) 0.0252(6) Uani 1 1 d . . . C6 C 1.0091(3) 0.7181(3) 0.59924(16) 0.0293(6) Uani 1 1 d . . . H6A H 1.0609 0.6570 0.5703 0.035 Uiso 1 1 calc R . . H6B H 1.0456 0.7905 0.5822 0.035 Uiso 1 1 calc R . . C7 C 1.0666(4) 0.3896(3) 0.6901(2) 0.0403(8) Uani 1 1 d . . . H7A H 1.0022 0.3790 0.7354 0.048 Uiso 1 1 calc R . . C8 C 0.9657(5) 0.4328(4) 0.6163(2) 0.0604(11) Uani 1 1 d . . . H8A H 0.9170 0.3706 0.6183 0.091 Uiso 1 1 calc R . . H8B H 1.0228 0.4412 0.5692 0.091 Uiso 1 1 calc R . . H8C H 0.8912 0.5147 0.6131 0.091 Uiso 1 1 calc R . . C9 C 1.1784(4) 0.2567(3) 0.7006(2) 0.0449(8) Uani 1 1 d . . . H9A H 1.1269 0.2006 0.6936 0.067 Uiso 1 1 calc R . . H9B H 1.2287 0.2235 0.7542 0.067 Uiso 1 1 calc R . . H9C H 1.2510 0.2614 0.6607 0.067 Uiso 1 1 calc R . . C10 C 1.3346(3) 0.4811(3) 0.64989(19) 0.0354(7) Uani 1 1 d . . . H10A H 1.4048 0.3953 0.6781 0.043 Uiso 1 1 calc R . . C11 C 1.4128(4) 0.5723(4) 0.6566(3) 0.0594(11) Uani 1 1 d . . . H11A H 1.5109 0.5475 0.6368 0.089 Uiso 1 1 calc R . . H11B H 1.4222 0.5698 0.7126 0.089 Uiso 1 1 calc R . . H11C H 1.3554 0.6583 0.6247 0.089 Uiso 1 1 calc R . . C12 C 1.3218(4) 0.4821(4) 0.5620(2) 0.0536(10) Uani 1 1 d . . . H12A H 1.4205 0.4498 0.5443 0.080 Uiso 1 1 calc R . . H12B H 1.2719 0.5688 0.5284 0.080 Uiso 1 1 calc R . . H12C H 1.2649 0.4284 0.5576 0.080 Uiso 1 1 calc R . . C13 C 1.2272(3) 0.4384(3) 0.81887(18) 0.0324(7) Uani 1 1 d . . . H13A H 1.2227 0.5153 0.8341 0.039 Uiso 1 1 calc R . . C14 C 1.3876(4) 0.3482(4) 0.8408(2) 0.0514(10) Uani 1 1 d . . . H14A H 1.4094 0.3233 0.8986 0.077 Uiso 1 1 calc R . . H14B H 1.4548 0.3912 0.8136 0.077 Uiso 1 1 calc R . . H14C H 1.4005 0.2728 0.8240 0.077 Uiso 1 1 calc R . . C15 C 1.1282(4) 0.3786(3) 0.8743(2) 0.0452(9) Uani 1 1 d . . . H15A H 1.1538 0.3711 0.9296 0.068 Uiso 1 1 calc R . . H15B H 1.1423 0.2945 0.8692 0.068 Uiso 1 1 calc R . . H15C H 1.0250 0.4319 0.8594 0.068 Uiso 1 1 calc R . . C16 C 1.3562(3) 0.7005(3) 0.86500(17) 0.0278(6) Uani 1 1 d . . . H16A H 1.4156 0.7163 0.8218 0.033 Uiso 1 1 calc R . . C17 C 1.4190(3) 0.6596(3) 0.94155(18) 0.0317(7) Uani 1 1 d . . . H17A H 1.5201 0.6474 0.9511 0.038 Uiso 1 1 calc R . . C18 C 1.3328(3) 0.6365(3) 1.00454(18) 0.0325(7) Uani 1 1 d . . . H18A H 1.3739 0.6079 1.0581 0.039 Uiso 1 1 calc R . . C19 C 1.1863(3) 0.6556(3) 0.98851(16) 0.0274(6) Uani 1 1 d . . . H19A H 1.1255 0.6396 1.0309 0.033 Uiso 1 1 calc R . . C20 C 1.1291(3) 0.6982(3) 0.91039(16) 0.0227(6) Uani 1 1 d . . . C21 C 0.9705(3) 0.7184(3) 0.88793(16) 0.0242(6) Uani 1 1 d . . . H21A H 0.9604 0.6358 0.8913 0.029 Uiso 1 1 calc R . . H21B H 0.9073 0.7530 0.9269 0.029 Uiso 1 1 calc R . . C22 C 0.8131(3) 1.0767(3) 0.70243(19) 0.0345(7) Uani 1 1 d . . . H22A H 0.9123 1.0869 0.6996 0.041 Uiso 1 1 calc R . . C23 C 0.7012(4) 1.2085(3) 0.6945(2) 0.0568(11) Uani 1 1 d . . . H23A H 0.7120 1.2682 0.6444 0.085 Uiso 1 1 calc R . . H23B H 0.7189 1.2367 0.7395 0.085 Uiso 1 1 calc R . . H23C H 0.6012 1.2046 0.6943 0.085 Uiso 1 1 calc R . . C24 C 0.7898(4) 1.0381(3) 0.62906(19) 0.0427(8) Uani 1 1 d . . . H24A H 0.7975 1.1027 0.5807 0.064 Uiso 1 1 calc R . . H24B H 0.6920 1.0300 0.6279 0.064 Uiso 1 1 calc R . . H24C H 0.8651 0.9569 0.6315 0.064 Uiso 1 1 calc R . . C25 C 0.9070(3) 1.0061(3) 0.88177(19) 0.0355(7) Uani 1 1 d . . . H25A H 0.9395 0.9290 0.9291 0.043 Uiso 1 1 calc R . . C26 C 0.8059(4) 1.1131(4) 0.9123(2) 0.0563(10) Uani 1 1 d . . . H26A H 0.8604 1.1248 0.9542 0.084 Uiso 1 1 calc R . . H26B H 0.7204 1.0909 0.9341 0.084 Uiso 1 1 calc R . . H26C H 0.7727 1.1916 0.8681 0.084 Uiso 1 1 calc R . . C27 C 1.0453(4) 1.0368(4) 0.8544(2) 0.0476(9) Uani 1 1 d . . . H27A H 1.0995 1.0392 0.9000 0.071 Uiso 1 1 calc R . . H27B H 1.0176 1.1193 0.8136 0.071 Uiso 1 1 calc R . . H27C H 1.1077 0.9717 0.8319 0.071 Uiso 1 1 calc R . . C28 C 0.6200(3) 0.9788(3) 0.83326(19) 0.0348(7) Uani 1 1 d . . . H28A H 0.5727 1.0677 0.8348 0.042 Uiso 1 1 calc R . . C29 C 0.5244(3) 0.9590(4) 0.7736(2) 0.0460(9) Uani 1 1 d . . . H29A H 0.4238 0.9753 0.7904 0.069 Uiso 1 1 calc R . . H29B H 0.5648 0.8717 0.7715 0.069 Uiso 1 1 calc R . . H29C H 0.5233 1.0172 0.7206 0.069 Uiso 1 1 calc R . . C30 C 0.6124(4) 0.8926(4) 0.9168(2) 0.0481(9) Uani 1 1 d . . . H30A H 0.5100 0.9137 0.9310 0.072 Uiso 1 1 calc R . . H30B H 0.6725 0.9051 0.9558 0.072 Uiso 1 1 calc R . . H30C H 0.6498 0.8042 0.9168 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0206(2) 0.0264(2) 0.0205(2) -0.00562(16) 0.00282(15) -0.00918(16) Fe2 0.01895(19) 0.0292(2) 0.0200(2) -0.00701(17) 0.00248(15) -0.00872(16) Cl1 0.0378(4) 0.0357(4) 0.0359(4) -0.0034(3) 0.0093(3) -0.0193(3) Cl2 0.0292(4) 0.0458(5) 0.0331(4) 0.0010(3) 0.0036(3) -0.0188(3) Si1 0.0224(4) 0.0251(4) 0.0309(4) -0.0106(3) 0.0027(3) -0.0053(3) Si2 0.0236(4) 0.0269(4) 0.0266(4) -0.0109(3) 0.0068(3) -0.0085(3) N1 0.0237(12) 0.0297(13) 0.0236(12) -0.0079(10) 0.0001(9) -0.0083(10) N2 0.0217(11) 0.0277(12) 0.0206(11) -0.0066(10) 0.0019(9) -0.0087(9) N3 0.0213(11) 0.0254(12) 0.0227(12) -0.0048(10) 0.0005(9) -0.0075(9) N4 0.0196(11) 0.0251(12) 0.0211(11) -0.0069(10) 0.0013(9) -0.0059(9) C1 0.0238(14) 0.0348(17) 0.0321(16) -0.0091(13) -0.0009(12) -0.0105(12) C2 0.0294(15) 0.0350(17) 0.0366(17) -0.0089(14) -0.0093(13) -0.0062(13) C3 0.0411(18) 0.0398(19) 0.0255(15) -0.0077(14) -0.0098(13) -0.0023(14) C4 0.0369(16) 0.0319(16) 0.0222(14) -0.0072(13) 0.0012(12) -0.0073(13) C5 0.0286(14) 0.0234(14) 0.0238(14) -0.0068(12) 0.0033(11) -0.0093(11) C6 0.0272(15) 0.0386(17) 0.0233(14) -0.0105(13) 0.0048(12) -0.0118(13) C7 0.0427(18) 0.0364(18) 0.0449(19) -0.0149(16) -0.0007(15) -0.0145(15) C8 0.068(3) 0.057(3) 0.064(3) -0.020(2) -0.006(2) -0.030(2) C9 0.061(2) 0.0366(19) 0.046(2) -0.0197(16) 0.0081(17) -0.0208(17) C10 0.0289(16) 0.0336(17) 0.0415(18) -0.0121(14) 0.0136(14) -0.0074(13) C11 0.038(2) 0.056(2) 0.093(3) -0.028(2) 0.030(2) -0.0234(18) C12 0.052(2) 0.061(2) 0.044(2) -0.0177(19) 0.0263(18) -0.0140(19) C13 0.0335(16) 0.0268(16) 0.0334(16) -0.0106(13) 0.0004(13) -0.0039(12) C14 0.0366(18) 0.059(2) 0.045(2) -0.0096(18) -0.0092(16) -0.0032(17) C15 0.0426(19) 0.047(2) 0.0330(17) -0.0038(16) 0.0034(15) -0.0057(16) C16 0.0228(14) 0.0295(16) 0.0315(16) -0.0084(13) 0.0025(12) -0.0097(12) C17 0.0216(14) 0.0334(17) 0.0376(17) -0.0075(14) -0.0053(12) -0.0081(12) C18 0.0317(16) 0.0363(17) 0.0257(15) -0.0049(13) -0.0076(12) -0.0094(13) C19 0.0285(14) 0.0324(16) 0.0210(14) -0.0074(12) 0.0023(11) -0.0105(12) C20 0.0232(13) 0.0219(14) 0.0247(14) -0.0079(11) 0.0026(11) -0.0088(11) C21 0.0229(13) 0.0278(15) 0.0224(14) -0.0070(12) 0.0026(11) -0.0097(11) C22 0.0316(16) 0.0294(16) 0.0382(17) -0.0064(14) 0.0014(13) -0.0077(13) C23 0.063(2) 0.0297(19) 0.057(2) 0.0009(17) 0.007(2) -0.0015(17) C24 0.0445(19) 0.0385(19) 0.0354(18) -0.0001(15) -0.0061(15) -0.0100(15) C25 0.0411(17) 0.0315(17) 0.0360(17) -0.0146(14) -0.0002(14) -0.0105(14) C26 0.061(2) 0.051(2) 0.065(3) -0.038(2) -0.002(2) -0.0100(19) C27 0.051(2) 0.050(2) 0.054(2) -0.0191(18) -0.0006(17) -0.0279(18) C28 0.0259(15) 0.0308(17) 0.0455(19) -0.0154(15) 0.0056(13) -0.0035(12) C29 0.0294(16) 0.050(2) 0.057(2) -0.0144(18) 0.0004(15) -0.0115(15) C30 0.0349(18) 0.060(2) 0.048(2) -0.0166(18) 0.0180(16) -0.0143(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.050(2) . ? Fe1 N3 2.092(2) . ? Fe1 N4 2.109(2) . ? Fe1 Cl1 2.2525(10) . ? Fe1 Fe2 2.7543(7) . ? Fe2 N4 2.039(2) . ? Fe2 N1 2.078(2) . ? Fe2 N2 2.102(2) . ? Fe2 Cl2 2.2583(10) . ? Si1 N4 1.771(2) . ? Si1 C22 1.891(3) . ? Si1 C28 1.895(3) . ? Si1 C25 1.914(3) . ? Si2 N2 1.766(2) . ? Si2 C7 1.897(4) . ? Si2 C10 1.897(3) . ? Si2 C13 1.905(3) . ? N1 C5 1.340(3) . ? N1 C1 1.354(3) . ? N2 C6 1.489(4) . ? N3 C16 1.346(3) . ? N3 C20 1.344(3) . ? N4 C21 1.496(3) . ? C1 C2 1.365(4) . ? C2 C3 1.381(4) . ? C3 C4 1.380(4) . ? C4 C5 1.386(4) . ? C5 C6 1.515(4) . ? C7 C8 1.499(5) . ? C7 C9 1.539(4) . ? C10 C11 1.527(5) . ? C10 C12 1.547(5) . ? C13 C15 1.531(4) . ? C13 C14 1.544(4) . ? C16 C17 1.372(4) . ? C17 C18 1.382(4) . ? C18 C19 1.379(4) . ? C19 C20 1.377(4) . ? C20 C21 1.513(4) . ? C22 C24 1.527(5) . ? C22 C23 1.537(4) . ? C25 C27 1.522(5) . ? C25 C26 1.539(4) . ? C28 C29 1.527(5) . ? C28 C30 1.537(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 N2 Fe1 N3 124.54(9) . . ? N2 Fe1 N4 96.36(9) . . ? N3 Fe1 N4 81.47(9) . . ? N2 Fe1 Cl1 117.01(7) . . ? N3 Fe1 Cl1 103.74(7) . . ? N4 Fe1 Cl1 131.46(7) . . ? N2 Fe1 Fe2 49.25(6) . . ? N3 Fe1 Fe2 110.87(7) . . ? N4 Fe1 Fe2 47.31(7) . . ? Cl1 Fe1 Fe2 143.58(3) . . ? N4 Fe2 N1 128.90(9) . . ? N4 Fe2 N2 96.92(9) . . ? N1 Fe2 N2 82.44(9) . . ? N4 Fe2 Cl2 115.53(7) . . ? N1 Fe2 Cl2 101.05(7) . . ? N2 Fe2 Cl2 131.55(7) . . ? N4 Fe2 Fe1 49.50(6) . . ? N1 Fe2 Fe1 108.44(7) . . ? N2 Fe2 Fe1 47.63(7) . . ? Cl2 Fe2 Fe1 149.32(3) . . ? N4 Si1 C22 110.37(12) . . ? N4 Si1 C28 111.88(13) . . ? C22 Si1 C28 110.74(14) . . ? N4 Si1 C25 108.23(13) . . ? C22 Si1 C25 108.72(15) . . ? C28 Si1 C25 106.75(14) . . ? N2 Si2 C7 112.97(13) . . ? N2 Si2 C10 111.64(13) . . ? C7 Si2 C10 109.55(15) . . ? N2 Si2 C13 107.75(12) . . ? C7 Si2 C13 106.95(15) . . ? C10 Si2 C13 107.74(14) . . ? C5 N1 C1 118.8(2) . . ? C5 N1 Fe2 114.30(18) . . ? C1 N1 Fe2 126.78(19) . . ? C6 N2 Si2 112.56(18) . . ? C6 N2 Fe1 110.09(18) . . ? Si2 N2 Fe1 119.65(12) . . ? C6 N2 Fe2 108.74(16) . . ? Si2 N2 Fe2 119.22(12) . . ? Fe1 N2 Fe2 83.12(8) . . ? C16 N3 C20 118.8(2) . . ? C16 N3 Fe1 127.39(18) . . ? C20 N3 Fe1 113.80(18) . . ? C21 N4 Si1 113.72(17) . . ? C21 N4 Fe2 104.35(17) . . ? Si1 N4 Fe2 125.94(12) . . ? C21 N4 Fe1 105.85(15) . . ? Si1 N4 Fe1 118.95(12) . . ? Fe2 N4 Fe1 83.19(8) . . ? N1 C1 C2 122.3(3) . . ? C1 C2 C3 119.0(3) . . ? C2 C3 C4 119.4(3) . . ? C3 C4 C5 118.9(3) . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 117.0(2) . . ? C4 C5 C6 121.4(2) . . ? N2 C6 C5 114.8(2) . . ? C8 C7 C9 111.1(3) . . ? C8 C7 Si2 119.5(3) . . ? C9 C7 Si2 109.8(2) . . ? C11 C10 C12 110.0(3) . . ? C11 C10 Si2 112.5(2) . . ? C12 C10 Si2 118.6(2) . . ? C15 C13 C14 108.0(3) . . ? C15 C13 Si2 115.3(2) . . ? C14 C13 Si2 115.6(2) . . ? N3 C16 C17 122.2(3) . . ? C16 C17 C18 119.0(3) . . ? C19 C18 C17 119.0(3) . . ? C20 C19 C18 119.4(3) . . ? N3 C20 C19 121.6(2) . . ? N3 C20 C21 115.8(2) . . ? C19 C20 C21 122.5(2) . . ? N4 C21 C20 113.1(2) . . ? C24 C22 C23 108.6(3) . . ? C24 C22 Si1 117.9(2) . . ? C23 C22 Si1 111.2(2) . . ? C27 C25 C26 108.9(3) . . ? C27 C25 Si1 113.2(2) . . ? C26 C25 Si1 115.1(2) . . ? C29 C28 C30 108.6(3) . . ? C29 C28 Si1 114.2(2) . . ? C30 C28 Si1 113.7(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.814 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.075 #=== END data_FO2974 _database_code_depnum_ccdc_archive 'CCDC 676623' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 Cl2 Fe2 N4 Si2 * 0.5 C4 H8 O' _chemical_formula_weight 949.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.0652(8) _cell_length_b 14.6411(7) _cell_length_c 16.8566(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.800(3) _cell_angle_gamma 90.00 _cell_volume 4787.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 16771 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16771 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5453 _reflns_number_gt 3358 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5453 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.67955(2) 0.25918(3) -0.03445(3) 0.02983(19) Uani 1 1 d . . . Si Si 0.73532(5) 0.05227(7) 0.01399(6) 0.0317(3) Uani 1 1 d . . . Cl Cl 0.57409(5) 0.26973(7) -0.01068(7) 0.0464(3) Uani 1 1 d . . . N1 N 0.65384(18) 0.2330(2) -0.16031(19) 0.0417(8) Uani 1 1 d . . . N2 N 0.75050(14) 0.1524(2) -0.03427(17) 0.0294(6) Uani 1 1 d . . . C1 C 0.5992(3) 0.2662(3) -0.2158(3) 0.0585(13) Uani 1 1 d . . . H1A H 0.5685 0.3057 -0.1979 0.070 Uiso 1 1 calc R . . C2 C 0.5861(3) 0.2450(4) -0.2979(3) 0.082(2) Uani 1 1 d . . . H2A H 0.5471 0.2697 -0.3363 0.098 Uiso 1 1 calc R . . C3 C 0.6303(3) 0.1878(4) -0.3227(3) 0.091(2) Uani 1 1 d . . . H3A H 0.6224 0.1726 -0.3791 0.109 Uiso 1 1 calc R . . C4 C 0.6863(3) 0.1520(4) -0.2667(3) 0.0759(18) Uani 1 1 d . . . H4A H 0.7170 0.1117 -0.2838 0.091 Uiso 1 1 calc R . . C5 C 0.6971(2) 0.1759(3) -0.1848(2) 0.0432(10) Uani 1 1 d . . . C6 C 0.7580(2) 0.1418(3) -0.1199(2) 0.0355(9) Uani 1 1 d . . . H6A H 0.7652 0.0763 -0.1301 0.043 Uiso 1 1 calc R . . H6B H 0.7997 0.1753 -0.1247 0.043 Uiso 1 1 calc R . . C7 C 0.6502(2) -0.0022(3) -0.0356(2) 0.0384(9) Uani 1 1 d . . . C8 C 0.6310(3) -0.0202(5) -0.1180(3) 0.088(2) Uani 1 1 d . . . H8A H 0.6605 -0.0015 -0.1510 0.105 Uiso 1 1 calc R . . C9 C 0.5687(3) -0.0657(5) -0.1556(4) 0.102(3) Uani 1 1 d . . . H9A H 0.5557 -0.0743 -0.2134 0.123 Uiso 1 1 calc R . . C10 C 0.5278(2) -0.0967(4) -0.1091(4) 0.0700(16) Uani 1 1 d . . . H10A H 0.4868 -0.1292 -0.1338 0.084 Uiso 1 1 calc R . . C11 C 0.5454(2) -0.0814(3) -0.0273(4) 0.0583(13) Uani 1 1 d . . . H11A H 0.5165 -0.1028 0.0054 0.070 Uiso 1 1 calc R . . C12 C 0.6062(2) -0.0339(3) 0.0093(3) 0.0482(11) Uani 1 1 d . . . H12A H 0.6174 -0.0233 0.0668 0.058 Uiso 1 1 calc R . . C13 C 0.7387(2) 0.0795(3) 0.1238(2) 0.0401(9) Uani 1 1 d . . . C14 C 0.6880(3) 0.1277(3) 0.1474(3) 0.0536(12) Uani 1 1 d . . . H14A H 0.6483 0.1470 0.1068 0.064 Uiso 1 1 calc R . . C15 C 0.6936(3) 0.1486(4) 0.2286(3) 0.0784(18) Uani 1 1 d . . . H15A H 0.6578 0.1817 0.2432 0.094 Uiso 1 1 calc R . . C16 C 0.7505(4) 0.1219(4) 0.2889(3) 0.091(2) Uani 1 1 d . . . H16A H 0.7540 0.1369 0.3447 0.109 Uiso 1 1 calc R . . C17 C 0.8012(3) 0.0743(4) 0.2682(3) 0.0724(16) Uani 1 1 d . . . H17A H 0.8404 0.0555 0.3097 0.087 Uiso 1 1 calc R . . C18 C 0.7965(2) 0.0524(3) 0.1859(2) 0.0495(11) Uani 1 1 d . . . H18A H 0.8326 0.0191 0.1721 0.059 Uiso 1 1 calc R . . C19 C 0.80297(19) -0.0357(2) 0.0124(2) 0.0335(8) Uani 1 1 d . . . C20 C 0.7934(2) -0.1264(3) 0.0354(3) 0.0425(10) Uani 1 1 d . . . H20A H 0.7519 -0.1423 0.0492 0.051 Uiso 1 1 calc R . . C21 C 0.8428(2) -0.1924(3) 0.0385(3) 0.0468(10) Uani 1 1 d . . . H21A H 0.8351 -0.2528 0.0548 0.056 Uiso 1 1 calc R . . C22 C 0.9038(2) -0.1715(3) 0.0181(3) 0.0458(10) Uani 1 1 d . . . H22A H 0.9378 -0.2171 0.0200 0.055 Uiso 1 1 calc R . . C23 C 0.9139(2) -0.0834(3) -0.0050(3) 0.0435(10) Uani 1 1 d . . . H23A H 0.9554 -0.0686 -0.0196 0.052 Uiso 1 1 calc R . . C24 C 0.86554(18) -0.0166(3) -0.0074(2) 0.0382(9) Uani 1 1 d . . . H24A H 0.8744 0.0438 -0.0227 0.046 Uiso 1 1 calc R . . O1T O 1.0000 -0.1714(10) 0.2500 0.107(4) Uiso 0.50 2 d SP . . C1T C 0.9557(7) -0.1064(9) 0.2833(8) 0.086(4) Uiso 0.50 1 d P . . H1TA H 0.9069 -0.1117 0.2519 0.104 Uiso 0.50 1 calc PR . . H1TB H 0.9589 -0.1200 0.3417 0.104 Uiso 0.50 1 calc PR . . C2T C 0.9811(6) -0.0166(9) 0.2750(7) 0.084(3) Uiso 0.50 1 d P . . H2TA H 0.9418 0.0256 0.2552 0.100 Uiso 0.50 1 calc PR . . H2TB H 1.0081 0.0053 0.3293 0.100 Uiso 0.50 1 calc PR . . 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 0.0289(3) 0.0309(3) 0.0314(3) -0.0063(2) 0.0110(2) -0.0039(2) Si 0.0335(5) 0.0279(6) 0.0359(5) -0.0032(4) 0.0130(4) -0.0051(4) Cl 0.0327(5) 0.0481(6) 0.0635(7) -0.0037(5) 0.0220(5) -0.0053(4) N1 0.0440(19) 0.044(2) 0.0351(17) -0.0096(14) 0.0058(15) 0.0033(15) N2 0.0343(16) 0.0282(16) 0.0269(14) -0.0054(12) 0.0100(12) -0.0039(13) C1 0.052(3) 0.069(3) 0.044(3) -0.015(2) -0.008(2) 0.016(2) C2 0.091(4) 0.096(5) 0.042(3) -0.014(3) -0.014(3) 0.037(3) C3 0.125(5) 0.095(5) 0.036(3) -0.023(3) -0.011(3) 0.052(4) C4 0.104(4) 0.079(4) 0.037(2) -0.018(2) 0.003(3) 0.040(3) C5 0.055(2) 0.040(2) 0.032(2) -0.0091(17) 0.0066(18) 0.0073(19) C6 0.045(2) 0.033(2) 0.0316(18) -0.0038(15) 0.0153(17) 0.0046(17) C7 0.0338(19) 0.027(2) 0.055(2) -0.0048(17) 0.0135(17) -0.0036(16) C8 0.086(4) 0.120(5) 0.068(3) -0.048(3) 0.038(3) -0.065(4) C9 0.088(4) 0.143(7) 0.076(4) -0.052(4) 0.022(3) -0.070(4) C10 0.043(3) 0.064(3) 0.100(4) -0.038(3) 0.012(3) -0.017(2) C11 0.033(2) 0.048(3) 0.097(4) 0.004(3) 0.023(2) -0.004(2) C12 0.035(2) 0.048(3) 0.060(3) 0.011(2) 0.0097(19) -0.0063(19) C13 0.050(2) 0.036(2) 0.040(2) 0.0010(17) 0.0218(19) -0.0064(18) C14 0.078(3) 0.043(3) 0.051(2) 0.010(2) 0.038(2) 0.014(2) C15 0.127(5) 0.072(4) 0.054(3) 0.013(3) 0.055(3) 0.027(4) C16 0.172(7) 0.075(4) 0.040(3) 0.006(3) 0.055(4) 0.013(4) C17 0.112(4) 0.071(4) 0.035(2) 0.002(2) 0.019(3) -0.007(3) C18 0.061(3) 0.053(3) 0.036(2) 0.0026(19) 0.015(2) -0.006(2) C19 0.0353(19) 0.029(2) 0.0357(19) -0.0020(15) 0.0083(15) -0.0036(16) C20 0.040(2) 0.035(2) 0.055(2) 0.0018(18) 0.0176(19) -0.0067(17) C21 0.050(2) 0.031(2) 0.060(3) 0.0032(18) 0.016(2) 0.0019(19) C22 0.036(2) 0.040(2) 0.060(3) -0.003(2) 0.0107(19) 0.0046(18) C23 0.034(2) 0.046(3) 0.051(2) -0.0009(19) 0.0122(18) -0.0007(18) C24 0.035(2) 0.035(2) 0.044(2) -0.0003(17) 0.0101(17) -0.0069(17) _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 N2 2.039(3) 7_655 ? Fe N1 2.087(3) . ? Fe N2 2.114(3) . ? Fe Cl 2.2573(11) . ? Fe Fe 2.7814(10) 7_655 ? Si N2 1.741(3) . ? Si C7 1.876(4) . ? Si C19 1.877(4) . ? Si C13 1.878(4) . ? N1 C1 1.337(5) . ? N1 C5 1.343(5) . ? N2 C6 1.498(4) . ? N2 Fe 2.039(3) 7_655 ? C1 C2 1.378(7) . ? C2 C3 1.361(7) . ? C3 C4 1.373(7) . ? C4 C5 1.387(5) . ? C5 C6 1.503(5) . ? C7 C8 1.368(6) . ? C7 C12 1.383(6) . ? C8 C9 1.415(7) . ? C9 C10 1.350(8) . ? C10 C11 1.351(7) . ? C11 C12 1.403(6) . ? C13 C14 1.378(6) . ? C13 C18 1.407(6) . ? C14 C15 1.379(6) . ? C15 C16 1.377(8) . ? C16 C17 1.352(8) . ? C17 C18 1.403(6) . ? C19 C24 1.407(5) . ? C19 C20 1.409(5) . ? C20 C21 1.376(6) . ? C21 C22 1.387(6) . ? C22 C23 1.378(6) . ? C23 C24 1.372(6) . ? O1T C1T 1.506(15) . ? O1T C1T 1.506(15) 2_755 ? C1T C2T 1.429(17) . ? C2T C2T 1.27(2) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe N1 130.53(13) 7_655 . ? N2 Fe N2 95.91(11) 7_655 . ? N1 Fe N2 81.78(12) . . ? N2 Fe Cl 113.34(9) 7_655 . ? N1 Fe Cl 101.16(10) . . ? N2 Fe Cl 135.40(9) . . ? N2 Fe Fe 49.10(8) 7_655 7_655 ? N1 Fe Fe 111.57(10) . 7_655 ? N2 Fe Fe 46.81(7) . 7_655 ? Cl Fe Fe 146.25(4) . 7_655 ? N2 Si C7 113.43(16) . . ? N2 Si C19 110.96(16) . . ? C7 Si C19 106.32(16) . . ? N2 Si C13 108.37(16) . . ? C7 Si C13 109.23(18) . . ? C19 Si C13 108.42(18) . . ? C1 N1 C5 119.3(3) . . ? C1 N1 Fe 126.1(3) . . ? C5 N1 Fe 114.5(3) . . ? C6 N2 Si 115.8(2) . . ? C6 N2 Fe 112.9(2) . 7_655 ? Si N2 Fe 116.52(15) . 7_655 ? C6 N2 Fe 108.0(2) . . ? Si N2 Fe 115.17(15) . . ? Fe N2 Fe 84.09(11) 7_655 . ? N1 C1 C2 122.3(5) . . ? C3 C2 C1 118.3(5) . . ? C2 C3 C4 120.5(4) . . ? C3 C4 C5 118.7(5) . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C6 117.0(3) . . ? C4 C5 C6 122.1(4) . . ? N2 C6 C5 113.7(3) . . ? C8 C7 C12 115.9(4) . . ? C8 C7 Si 121.5(3) . . ? C12 C7 Si 122.3(3) . . ? C7 C8 C9 122.2(5) . . ? C10 C9 C8 119.7(5) . . ? C9 C10 C11 119.8(4) . . ? C10 C11 C12 120.2(5) . . ? C7 C12 C11 122.0(4) . . ? C14 C13 C18 117.4(4) . . ? C14 C13 Si 123.3(3) . . ? C18 C13 Si 119.3(3) . . ? C13 C14 C15 121.3(5) . . ? C16 C15 C14 120.9(5) . . ? C17 C16 C15 119.5(5) . . ? C16 C17 C18 120.6(5) . . ? C17 C18 C13 120.4(5) . . ? C24 C19 C20 116.5(4) . . ? C24 C19 Si 124.0(3) . . ? C20 C19 Si 119.5(3) . . ? C21 C20 C19 121.7(4) . . ? C20 C21 C22 120.5(4) . . ? C23 C22 C21 118.7(4) . . ? C24 C23 C22 121.4(4) . . ? C23 C24 C19 121.2(4) . . ? C1T O1T C1T 101.5(14) . 2_755 ? C2T C1T O1T 106.6(11) . . ? C2T C2T C1T 110.7(7) 2_755 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.894 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.089 #=== END data_FO3292 _database_code_depnum_ccdc_archive 'CCDC 676624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 Cl2 Fe N2 Si' _chemical_formula_weight 347.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.8690(9) _cell_length_b 13.2269(5) _cell_length_c 7.8214(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.908(3) _cell_angle_gamma 90.00 _cell_volume 1713.62(16) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 11398 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.51 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11398 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3899 _reflns_number_gt 2832 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0488P)^2^+1.6259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3899 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.82798(3) 0.04143(3) 0.56482(5) 0.03144(14) Uani 1 1 d . . . Cl1 Cl 0.84257(5) -0.12084(6) 0.49926(11) 0.0438(2) Uani 1 1 d . . . Cl2 Cl 0.79835(6) 0.15954(7) 0.35800(11) 0.0514(3) Uani 1 1 d . . . Si Si 0.66295(6) 0.04259(8) 0.76743(14) 0.0448(3) Uani 1 1 d . . . N1 N 0.92406(14) 0.09221(19) 0.7587(3) 0.0313(5) Uani 1 1 d . . . N2 N 0.76862(15) 0.06221(18) 0.7781(3) 0.0308(5) Uani 1 1 d . . . C1 C 1.00133(19) 0.1053(2) 0.7472(4) 0.0385(7) Uani 1 1 d . . . H1A H 1.0172 0.0924 0.6390 0.046 Uiso 1 1 calc R . . C2 C 1.0591(2) 0.1369(2) 0.8864(5) 0.0433(8) Uani 1 1 d . . . H2A H 1.1136 0.1454 0.8739 0.052 Uiso 1 1 calc R . . C3 C 1.0366(2) 0.1558(2) 1.0433(5) 0.0450(8) Uani 1 1 d . . . H3A H 1.0755 0.1768 1.1411 0.054 Uiso 1 1 calc R . . C4 C 0.9568(2) 0.1438(2) 1.0568(4) 0.0426(8) Uani 1 1 d . . . H4A H 0.9398 0.1571 1.1637 0.051 Uiso 1 1 calc R . . C5 C 0.90186(19) 0.1122(2) 0.9121(4) 0.0327(6) Uani 1 1 d . . . C6 C 0.81567(19) 0.0974(2) 0.9119(4) 0.0357(7) Uani 1 1 d . . . H6A H 0.7946 0.1142 1.0127 0.043 Uiso 1 1 calc R . . C7 C 0.6204(3) 0.1514(3) 0.8624(10) 0.108(2) Uani 1 1 d . . . H7A H 0.6380 0.1503 0.9892 0.162 Uiso 1 1 calc R . . H7B H 0.5613 0.1482 0.8334 0.162 Uiso 1 1 calc R . . H7C H 0.6390 0.2138 0.8154 0.162 Uiso 1 1 calc R . . C8 C 0.6223(3) 0.0304(5) 0.5264(6) 0.103(2) Uani 1 1 d . . . H8A H 0.6408 0.0879 0.4652 0.155 Uiso 1 1 calc R . . H8B H 0.5632 0.0296 0.5055 0.155 Uiso 1 1 calc R . . H8C H 0.6420 -0.0326 0.4834 0.155 Uiso 1 1 calc R . . C9 C 0.6490(2) -0.0795(3) 0.8797(5) 0.0467(8) Uani 1 1 d . . . C10 C 0.6996(3) -0.1634(3) 0.8292(7) 0.0761(14) Uani 1 1 d . . . H10A H 0.6912 -0.2248 0.8935 0.114 Uiso 1 1 calc R . . H10B H 0.7567 -0.1441 0.8573 0.114 Uiso 1 1 calc R . . H10C H 0.6841 -0.1761 0.7039 0.114 Uiso 1 1 calc R . . C11 C 0.5603(3) -0.1077(4) 0.8482(7) 0.0802(15) Uani 1 1 d . . . H11A H 0.5525 -0.1649 0.9229 0.120 Uiso 1 1 calc R . . H11B H 0.5425 -0.1267 0.7258 0.120 Uiso 1 1 calc R . . H11C H 0.5287 -0.0498 0.8754 0.120 Uiso 1 1 calc R . . C12 C 0.6758(4) -0.0634(4) 1.0788(6) 0.0881(17) Uani 1 1 d . . . H12A H 0.6611 -0.1229 1.1407 0.132 Uiso 1 1 calc R . . H12B H 0.6488 -0.0035 1.1145 0.132 Uiso 1 1 calc R . . H12C H 0.7344 -0.0537 1.1068 0.132 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 0.0327(2) 0.0384(3) 0.0240(2) -0.00225(18) 0.00738(17) -0.00188(18) Cl1 0.0463(5) 0.0429(5) 0.0439(5) -0.0083(4) 0.0131(4) 0.0028(3) Cl2 0.0807(7) 0.0447(5) 0.0295(4) 0.0029(3) 0.0127(4) -0.0006(4) Si 0.0284(5) 0.0563(6) 0.0519(6) 0.0182(5) 0.0135(4) 0.0057(4) N1 0.0310(13) 0.0351(13) 0.0282(13) -0.0006(11) 0.0068(10) -0.0005(10) N2 0.0288(13) 0.0358(14) 0.0293(13) 0.0018(10) 0.0092(10) 0.0003(10) C1 0.0322(16) 0.0450(18) 0.0390(17) 0.0008(15) 0.0082(13) 0.0007(13) C2 0.0310(17) 0.0436(19) 0.052(2) 0.0022(16) -0.0003(15) -0.0024(14) C3 0.042(2) 0.0420(19) 0.044(2) 0.0011(15) -0.0100(15) -0.0042(15) C4 0.058(2) 0.0381(18) 0.0296(16) -0.0031(14) 0.0043(15) -0.0077(15) C5 0.0385(17) 0.0305(15) 0.0299(15) -0.0007(12) 0.0086(13) -0.0022(12) C6 0.0428(18) 0.0398(17) 0.0278(15) -0.0024(13) 0.0149(13) -0.0025(14) C7 0.076(3) 0.061(3) 0.212(7) 0.022(4) 0.091(4) 0.023(2) C8 0.050(3) 0.196(7) 0.056(3) 0.050(4) -0.008(2) -0.024(3) C9 0.044(2) 0.050(2) 0.049(2) 0.0042(17) 0.0168(16) 0.0000(16) C10 0.084(3) 0.050(2) 0.105(4) 0.007(2) 0.045(3) 0.006(2) C11 0.047(2) 0.090(3) 0.103(4) 0.035(3) 0.014(2) -0.014(2) C12 0.138(5) 0.077(3) 0.046(2) 0.015(2) 0.010(3) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.109(2) . ? Fe N2 2.120(2) . ? Fe Cl1 2.2312(9) . ? Fe Cl2 2.2363(9) . ? Si N2 1.788(3) . ? Si C7 1.827(5) . ? Si C9 1.874(4) . ? Si C8 1.887(5) . ? N1 C1 1.335(4) . ? N1 C5 1.349(4) . ? N2 C6 1.276(4) . ? C1 C2 1.382(5) . ? C2 C3 1.374(5) . ? C3 C4 1.379(5) . ? C4 C5 1.385(4) . ? C5 C6 1.467(4) . ? C9 C10 1.499(5) . ? C9 C11 1.515(5) . ? C9 C12 1.551(6) . ? 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 78.82(9) . . ? N1 Fe Cl1 111.62(7) . . ? N2 Fe Cl1 113.25(7) . . ? N1 Fe Cl2 109.50(7) . . ? N2 Fe Cl2 113.85(7) . . ? Cl1 Fe Cl2 121.67(4) . . ? N2 Si C7 109.4(2) . . ? N2 Si C9 108.44(14) . . ? C7 Si C9 113.2(2) . . ? N2 Si C8 103.25(17) . . ? C7 Si C8 112.1(3) . . ? C9 Si C8 109.9(2) . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Fe 128.3(2) . . ? C5 N1 Fe 113.4(2) . . ? C6 N2 Si 123.4(2) . . ? C6 N2 Fe 112.3(2) . . ? Si N2 Fe 124.05(13) . . ? N1 C1 C2 122.6(3) . . ? C3 C2 C1 119.1(3) . . ? C2 C3 C4 119.1(3) . . ? C3 C4 C5 119.0(3) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 114.5(3) . . ? C4 C5 C6 123.5(3) . . ? N2 C6 C5 120.8(3) . . ? C10 C9 C11 111.6(4) . . ? C10 C9 C12 107.0(4) . . ? C11 C9 C12 106.8(4) . . ? C10 C9 Si 112.7(3) . . ? C11 C9 Si 110.1(3) . . ? C12 C9 Si 108.3(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.593 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.072 #=== END data_FO3279 _database_code_depnum_ccdc_archive 'CCDC 676625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Cl2 Fe N2 Si' _chemical_formula_weight 375.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2991(5) _cell_length_b 8.0232(5) _cell_length_c 17.7411(13) _cell_angle_alpha 81.560(5) _cell_angle_beta 80.001(4) _cell_angle_gamma 64.211(4) _cell_volume 918.29(11) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5715 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5715 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3947 _reflns_number_gt 3280 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0462P)^2^+1.5770P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3947 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.61170(6) 0.34805(6) 0.15240(2) 0.02818(13) Uani 1 1 d . . . Si Si 0.82872(14) 0.01992(12) 0.30332(5) 0.0347(2) Uani 1 1 d . . . Cl1 Cl 0.37342(13) 0.25001(12) 0.14299(5) 0.0440(2) Uani 1 1 d . . . Cl2 Cl 0.51541(13) 0.64829(11) 0.16575(6) 0.0468(2) Uani 1 1 d . . . N1 N 0.8534(4) 0.2816(3) 0.06220(14) 0.0290(5) Uani 1 1 d . . . N2 N 0.8509(4) 0.1229(3) 0.20689(13) 0.0277(5) Uani 1 1 d . . . C1 C 0.8548(5) 0.3653(4) -0.00891(17) 0.0340(6) Uani 1 1 d . . . H1A H 0.7365 0.4728 -0.0216 0.041 Uiso 1 1 calc R . . C2 C 1.0221(5) 0.3010(5) -0.06455(18) 0.0384(7) Uani 1 1 d . . . H2A H 1.0185 0.3640 -0.1144 0.046 Uiso 1 1 calc R . . C3 C 1.1936(5) 0.1449(5) -0.04696(19) 0.0376(7) Uani 1 1 d . . . H3A H 1.3089 0.0972 -0.0847 0.045 Uiso 1 1 calc R . . C4 C 1.1959(5) 0.0580(4) 0.02673(18) 0.0322(6) Uani 1 1 d . . . H4A H 1.3128 -0.0496 0.0405 0.039 Uiso 1 1 calc R . . C5 C 1.0241(4) 0.1316(4) 0.07961(16) 0.0280(6) Uani 1 1 d . . . C6 C 1.0129(4) 0.0515(4) 0.15983(17) 0.0299(6) Uani 1 1 d . . . H6A H 1.1275 -0.0543 0.1766 0.036 Uiso 1 1 calc R . . C7 C 1.0805(6) -0.1740(6) 0.3225(2) 0.0564(10) Uani 1 1 d . . . H7A H 1.1195 -0.2689 0.2865 0.085 Uiso 1 1 calc R . . H7B H 1.0687 -0.2289 0.3752 0.085 Uiso 1 1 calc R . . H7C H 1.1853 -0.1259 0.3159 0.085 Uiso 1 1 calc R . . C8 C 0.6350(7) -0.0724(6) 0.3029(2) 0.0586(11) Uani 1 1 d . . . H8A H 0.6866 -0.1664 0.2657 0.088 Uiso 1 1 calc R . . H8B H 0.5070 0.0292 0.2887 0.088 Uiso 1 1 calc R . . H8C H 0.6095 -0.1287 0.3542 0.088 Uiso 1 1 calc R . . C9 C 0.7362(5) 0.2009(5) 0.37543(18) 0.0407(8) Uani 1 1 d . . . C10 C 0.5326(8) 0.3612(8) 0.3585(3) 0.091(2) Uani 1 1 d . . . H10A H 0.4812 0.4453 0.3997 0.136 Uiso 1 1 calc R . . H10B H 0.4328 0.3120 0.3553 0.136 Uiso 1 1 calc R . . H10C H 0.5533 0.4291 0.3095 0.136 Uiso 1 1 calc R . . C11 C 0.7076(9) 0.0981(7) 0.4535(2) 0.0738(14) Uani 1 1 d . . . H11A H 0.6455 0.1869 0.4930 0.111 Uiso 1 1 calc R . . H11B H 0.8412 0.0040 0.4664 0.111 Uiso 1 1 calc R . . H11C H 0.6178 0.0377 0.4508 0.111 Uiso 1 1 calc R . . C12 C 0.9010(9) 0.2741(7) 0.3814(3) 0.0721(13) Uani 1 1 d . . . H12A H 1.0187 0.1630 0.4011 0.086 Uiso 1 1 calc R . . C13 C 0.8304(12) 0.4138(9) 0.4430(3) 0.103(2) Uani 1 1 d . . . H13A H 0.9444 0.4424 0.4490 0.155 Uiso 1 1 calc R . . H13B H 0.7864 0.3597 0.4919 0.155 Uiso 1 1 calc R . . H13C H 0.7157 0.5280 0.4270 0.155 Uiso 1 1 calc R . . C14 C 0.9879(10) 0.3430(11) 0.3128(4) 0.114(3) Uani 1 1 d . . . H14A H 1.0731 0.3986 0.3258 0.170 Uiso 1 1 calc R . . H14B H 0.8778 0.4372 0.2849 0.170 Uiso 1 1 calc R . . H14C H 1.0725 0.2406 0.2804 0.170 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 0.0244(2) 0.0274(2) 0.0288(2) -0.00157(16) -0.00342(16) -0.00733(17) Si 0.0328(5) 0.0353(4) 0.0280(4) 0.0029(3) -0.0056(3) -0.0080(4) Cl1 0.0354(4) 0.0495(5) 0.0522(5) 0.0028(4) -0.0122(4) -0.0221(4) Cl2 0.0400(5) 0.0287(4) 0.0615(5) -0.0074(3) 0.0043(4) -0.0077(3) N1 0.0282(13) 0.0290(12) 0.0282(12) -0.0037(9) -0.0027(9) -0.0104(10) N2 0.0262(12) 0.0275(12) 0.0275(12) -0.0009(9) -0.0072(9) -0.0084(10) C1 0.0379(17) 0.0325(15) 0.0293(15) -0.0009(12) -0.0044(12) -0.0132(13) C2 0.0475(19) 0.0423(18) 0.0278(15) -0.0018(13) 0.0000(13) -0.0232(15) C3 0.0359(17) 0.0431(17) 0.0380(17) -0.0142(14) 0.0064(13) -0.0212(14) C4 0.0280(15) 0.0356(16) 0.0356(16) -0.0084(12) -0.0033(12) -0.0142(13) C5 0.0270(14) 0.0302(14) 0.0300(14) -0.0058(11) -0.0047(11) -0.0135(12) C6 0.0261(14) 0.0296(14) 0.0315(15) -0.0035(11) -0.0067(11) -0.0082(11) C7 0.052(2) 0.048(2) 0.041(2) 0.0067(16) -0.0081(16) 0.0026(17) C8 0.072(3) 0.061(2) 0.053(2) 0.0155(19) -0.014(2) -0.041(2) C9 0.0368(17) 0.0476(19) 0.0241(14) 0.0008(13) -0.0017(12) -0.0071(14) C10 0.062(3) 0.093(4) 0.062(3) -0.030(3) -0.015(2) 0.028(3) C11 0.105(4) 0.075(3) 0.032(2) 0.0028(19) 0.010(2) -0.038(3) C12 0.093(4) 0.072(3) 0.060(3) -0.028(2) 0.011(2) -0.043(3) C13 0.161(6) 0.099(4) 0.072(4) -0.041(3) 0.021(4) -0.077(5) C14 0.108(5) 0.185(7) 0.105(5) -0.090(5) 0.049(4) -0.113(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe N1 2.100(2) . ? Fe N2 2.139(2) . ? Fe Cl2 2.2337(9) . ? Fe Cl1 2.2363(9) . ? Si N2 1.800(2) . ? Si C8 1.861(4) . ? Si C7 1.867(4) . ? Si C9 1.895(4) . ? N1 C5 1.348(4) . ? N1 C1 1.340(4) . ? N2 C6 1.278(4) . ? C1 C2 1.384(5) . ? C2 C3 1.375(5) . ? C3 C4 1.388(5) . ? C4 C5 1.382(4) . ? C5 C6 1.477(4) . ? C9 C10 1.527(5) . ? C9 C11 1.534(5) . ? C9 C12 1.575(6) . ? C12 C14 1.425(8) . ? C12 C13 1.541(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 78.91(9) . . ? N1 Fe Cl2 104.92(7) . . ? N2 Fe Cl2 124.91(7) . . ? N1 Fe Cl1 114.56(7) . . ? N2 Fe Cl1 107.24(7) . . ? Cl2 Fe Cl1 119.13(4) . . ? N2 Si C8 103.54(15) . . ? N2 Si C7 109.54(15) . . ? C8 Si C7 110.3(2) . . ? N2 Si C9 110.79(13) . . ? C8 Si C9 110.90(19) . . ? C7 Si C9 111.51(17) . . ? C5 N1 C1 117.9(3) . . ? C5 N1 Fe 113.75(19) . . ? C1 N1 Fe 128.3(2) . . ? C6 N2 Si 121.4(2) . . ? C6 N2 Fe 111.79(19) . . ? Si N2 Fe 126.38(13) . . ? N1 C1 C2 122.4(3) . . ? C3 C2 C1 119.3(3) . . ? C2 C3 C4 119.1(3) . . ? C5 C4 C3 118.4(3) . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 122.6(3) . . ? N2 C6 C5 120.7(3) . . ? C10 C9 C11 110.0(4) . . ? C10 C9 C12 111.1(4) . . ? C11 C9 C12 106.4(3) . . ? C10 C9 Si 111.3(3) . . ? C11 C9 Si 105.1(3) . . ? C12 C9 Si 112.7(3) . . ? C14 C12 C13 109.5(5) . . ? C14 C12 C9 118.5(4) . . ? C13 C12 C9 112.8(4) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.918 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.073 #=== END data_FO2873 _database_code_depnum_ccdc_archive 'CCDC 676626' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Cl4 Fe2 N4 Si2' _chemical_formula_weight 778.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7619(15) _cell_length_b 7.6925(5) _cell_length_c 15.8045(13) _cell_angle_alpha 90.00 _cell_angle_beta 112.645(3) _cell_angle_gamma 90.00 _cell_volume 1992.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12798 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour magenta _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12798 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4424 _reflns_number_gt 3588 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0530P)^2^+0.8262P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4424 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.324954(19) 0.86886(4) -0.00338(2) 0.03698(11) Uani 1 1 d . . . Cl1 Cl 0.42215(4) 0.95308(9) 0.12966(5) 0.05459(18) Uani 1 1 d . . . Cl2 Cl 0.24147(4) 1.05816(8) -0.10182(5) 0.05245(17) Uani 1 1 d . . . Si Si 0.18732(3) 0.57932(8) 0.03808(4) 0.03262(14) Uani 1 1 d . . . N1 N 0.38424(10) 0.7067(2) -0.06602(12) 0.0363(4) Uani 1 1 d . . . N2 N 0.26967(11) 0.6250(2) 0.00079(12) 0.0327(4) Uani 1 1 d . . . C1 C 0.44001(14) 0.7499(3) -0.09988(16) 0.0426(5) Uani 1 1 d . . . H1A H 0.4553 0.8685 -0.0987 0.051 Uiso 1 1 calc R . . C2 C 0.47645(15) 0.6277(4) -0.13670(17) 0.0477(6) Uani 1 1 d . . . H2A H 0.5154 0.6627 -0.1610 0.057 Uiso 1 1 calc R . . C3 C 0.45546(15) 0.4557(4) -0.13761(16) 0.0476(6) Uani 1 1 d . . . H3A H 0.4801 0.3699 -0.1618 0.057 Uiso 1 1 calc R . . C4 C 0.39735(15) 0.4090(3) -0.10231(16) 0.0435(5) Uani 1 1 d . . . H4A H 0.3815 0.2911 -0.1021 0.052 Uiso 1 1 calc R . . C5 C 0.36346(13) 0.5379(3) -0.06773(14) 0.0348(4) Uani 1 1 d . . . C6 C 0.30059(13) 0.5030(3) -0.03009(15) 0.0371(5) Uani 1 1 d . . . H6A H 0.2828 0.3870 -0.0289 0.044 Uiso 1 1 calc R . . C7 C 0.09175(14) 0.5675(3) -0.06943(16) 0.0419(5) Uani 1 1 d . . . H7A H 0.0460 0.5411 -0.0494 0.050 Uiso 1 1 calc R . . C8 C 0.09281(18) 0.4211(5) -0.1344(2) 0.0643(8) Uani 1 1 d . . . H8A H 0.0401 0.4167 -0.1863 0.096 Uiso 1 1 calc R . . H8B H 0.1029 0.3100 -0.1016 0.096 Uiso 1 1 calc R . . H8C H 0.1362 0.4429 -0.1570 0.096 Uiso 1 1 calc R . . C9 C 0.07072(17) 0.7411(4) -0.12121(19) 0.0601(7) Uani 1 1 d . . . H9A H 0.0198 0.7288 -0.1751 0.090 Uiso 1 1 calc R . . H9B H 0.1148 0.7741 -0.1408 0.090 Uiso 1 1 calc R . . H9C H 0.0641 0.8312 -0.0808 0.090 Uiso 1 1 calc R . . C10 C 0.18147(13) 0.7706(3) 0.10907(15) 0.0381(5) Uani 1 1 d . . . H10A H 0.1840 0.8768 0.0738 0.046 Uiso 1 1 calc R . . C11 C 0.09935(16) 0.7792(4) 0.1217(2) 0.0545(7) Uani 1 1 d . . . H11A H 0.0991 0.8810 0.1588 0.082 Uiso 1 1 calc R . . H11B H 0.0925 0.6736 0.1527 0.082 Uiso 1 1 calc R . . H11C H 0.0545 0.7883 0.0615 0.082 Uiso 1 1 calc R . . C12 C 0.25179(16) 0.7851(3) 0.20237(17) 0.0506(6) Uani 1 1 d . . . H12A H 0.2495 0.8983 0.2297 0.076 Uiso 1 1 calc R . . H12B H 0.3038 0.7740 0.1947 0.076 Uiso 1 1 calc R . . H12C H 0.2473 0.6923 0.2427 0.076 Uiso 1 1 calc R . . C13 C 0.21040(15) 0.3619(3) 0.09777(17) 0.0418(5) Uani 1 1 d . . . H13A H 0.2096 0.2754 0.0502 0.050 Uiso 1 1 calc R . . C14 C 0.29505(17) 0.3468(4) 0.17531(19) 0.0553(7) Uani 1 1 d . . . H14A H 0.3064 0.2246 0.1933 0.083 Uiso 1 1 calc R . . H14B H 0.2963 0.4152 0.2281 0.083 Uiso 1 1 calc R . . H14C H 0.3365 0.3908 0.1540 0.083 Uiso 1 1 calc R . . C15 C 0.14387(17) 0.3044(4) 0.1311(2) 0.0576(7) Uani 1 1 d . . . H15A H 0.1559 0.1868 0.1566 0.086 Uiso 1 1 calc R . . H15B H 0.0909 0.3049 0.0795 0.086 Uiso 1 1 calc R . . H15C H 0.1423 0.3847 0.1785 0.086 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 0.04206(19) 0.03021(18) 0.0444(2) -0.00301(12) 0.02299(15) -0.00463(12) Cl1 0.0558(4) 0.0593(4) 0.0521(4) -0.0152(3) 0.0246(3) -0.0192(3) Cl2 0.0671(4) 0.0317(3) 0.0592(4) 0.0029(2) 0.0251(3) 0.0046(3) Si 0.0319(3) 0.0323(3) 0.0350(3) 0.0002(2) 0.0143(2) -0.0030(2) N1 0.0333(9) 0.0390(10) 0.0387(10) -0.0016(8) 0.0163(8) -0.0024(7) N2 0.0345(9) 0.0303(9) 0.0340(9) -0.0002(7) 0.0141(7) -0.0030(7) C1 0.0366(11) 0.0488(13) 0.0451(13) -0.0005(10) 0.0188(10) -0.0035(10) C2 0.0374(12) 0.0679(17) 0.0417(13) -0.0023(11) 0.0196(10) 0.0019(11) C3 0.0436(13) 0.0604(16) 0.0402(13) -0.0066(11) 0.0177(11) 0.0121(11) C4 0.0460(13) 0.0427(13) 0.0408(13) -0.0031(10) 0.0155(10) 0.0041(10) C5 0.0359(11) 0.0359(11) 0.0310(11) -0.0018(8) 0.0112(9) 0.0006(8) C6 0.0392(11) 0.0324(11) 0.0402(12) -0.0005(9) 0.0159(9) -0.0030(9) C7 0.0336(11) 0.0492(14) 0.0411(13) 0.0010(10) 0.0123(9) -0.0039(9) C8 0.0469(15) 0.087(2) 0.0506(16) -0.0238(15) 0.0100(12) -0.0089(14) C9 0.0481(15) 0.0721(19) 0.0518(16) 0.0217(14) 0.0100(12) -0.0006(13) C10 0.0407(12) 0.0357(11) 0.0423(12) -0.0022(9) 0.0208(10) -0.0039(9) C11 0.0537(15) 0.0512(15) 0.0708(18) -0.0126(13) 0.0374(14) -0.0038(11) C12 0.0569(15) 0.0495(15) 0.0457(14) -0.0095(11) 0.0202(12) -0.0129(12) C13 0.0488(13) 0.0344(12) 0.0467(13) 0.0056(9) 0.0234(11) 0.0010(9) C14 0.0519(15) 0.0606(17) 0.0552(16) 0.0190(13) 0.0225(13) 0.0119(12) C15 0.0577(16) 0.0486(15) 0.0753(19) 0.0200(13) 0.0354(14) -0.0003(12) _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 2.1091(18) . ? Fe N2 2.1301(17) . ? Fe Cl2 2.2278(7) . ? Fe Cl1 2.2419(7) . ? Si N2 1.8094(18) . ? Si C10 1.877(2) . ? Si C7 1.886(2) . ? Si C13 1.886(2) . ? N1 C1 1.337(3) . ? N1 C5 1.347(3) . ? N2 C6 1.275(3) . ? C1 C2 1.390(3) . ? C2 C3 1.373(4) . ? C3 C4 1.396(4) . ? C4 C5 1.377(3) . ? C5 C6 1.478(3) . ? C7 C8 1.529(4) . ? C7 C9 1.536(4) . ? C10 C12 1.526(3) . ? C10 C11 1.548(3) . ? C13 C15 1.533(3) . ? C13 C14 1.535(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe N2 79.22(7) . . ? N1 Fe Cl2 112.16(5) . . ? N2 Fe Cl2 113.98(5) . . ? N1 Fe Cl1 105.54(5) . . ? N2 Fe Cl1 115.04(5) . . ? Cl2 Fe Cl1 122.09(3) . . ? N2 Si C10 106.27(9) . . ? N2 Si C7 106.02(9) . . ? C10 Si C7 109.80(11) . . ? N2 Si C13 106.73(9) . . ? C10 Si C13 116.57(11) . . ? C7 Si C13 110.78(11) . . ? C1 N1 C5 118.12(19) . . ? C1 N1 Fe 128.43(16) . . ? C5 N1 Fe 113.40(13) . . ? C6 N2 Si 120.20(15) . . ? C6 N2 Fe 111.37(14) . . ? Si N2 Fe 128.41(9) . . ? N1 C1 C2 122.4(2) . . ? C3 C2 C1 119.2(2) . . ? C2 C3 C4 118.9(2) . . ? C5 C4 C3 118.5(2) . . ? N1 C5 C4 122.9(2) . . ? N1 C5 C6 114.22(18) . . ? C4 C5 C6 122.9(2) . . ? N2 C6 C5 121.6(2) . . ? C8 C7 C9 110.2(2) . . ? C8 C7 Si 113.66(18) . . ? C9 C7 Si 112.83(17) . . ? C12 C10 C11 109.5(2) . . ? C12 C10 Si 114.96(17) . . ? C11 C10 Si 112.46(16) . . ? C15 C13 C14 110.6(2) . . ? C15 C13 Si 112.34(17) . . ? C14 C13 Si 115.10(17) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.364 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.056 # data_FO3694 _database_code_depnum_ccdc_archive 'CCDC 736365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 Cl4 Fe2 N4 Si2, 2(C4 H8 O) ' _chemical_formula_sum 'C28 H28 Cl2 Fe N2 O Si' _chemical_formula_weight 563.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 9.0029(4) _cell_length_b 18.7006(7) _cell_length_c 15.8978(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.290(2) _cell_angle_gamma 90.00 _cell_volume 2675.87(17) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 17985 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17985 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6082 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0561P)^2^+0.2222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6082 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.93546(4) 0.44098(2) 0.57976(2) 0.02364(12) Uani 1 1 d . . . Cl1 Cl 0.96493(8) 0.56663(3) 0.56788(4) 0.02788(16) Uani 1 1 d . . . Cl2 Cl 1.07254(8) 0.34893(4) 0.63183(4) 0.03482(18) Uani 1 1 d . . . Si1 Si 0.88310(8) 0.47117(4) 0.80300(4) 0.02304(17) Uani 1 1 d . . . N1 N 0.7128(3) 0.41712(12) 0.54137(13) 0.0271(5) Uani 1 1 d . . . N2 N 0.8145(2) 0.45177(11) 0.69900(13) 0.0233(5) Uani 1 1 d . . . C1 C 0.6601(3) 0.40312(17) 0.46392(17) 0.0376(7) Uani 1 1 d . . . H1A H 0.7272 0.4031 0.4187 0.045 Uiso 1 1 calc R . . C2 C 0.5109(4) 0.38863(19) 0.44682(19) 0.0451(8) Uani 1 1 d . . . H2A H 0.4773 0.3790 0.3909 0.054 Uiso 1 1 calc R . . C3 C 0.4125(3) 0.38839(18) 0.51185(19) 0.0411(8) Uani 1 1 d . . . H3A H 0.3100 0.3792 0.5014 0.049 Uiso 1 1 calc R . . C4 C 0.4654(3) 0.40177(17) 0.59267(18) 0.0354(7) Uani 1 1 d . . . H4A H 0.4002 0.4010 0.6388 0.043 Uiso 1 1 calc R . . C5 C 0.6149(3) 0.41621(15) 0.60506(16) 0.0262(6) Uani 1 1 d . . . C6 C 0.6796(3) 0.43200(15) 0.68886(17) 0.0280(6) Uani 1 1 d . . . H6A H 0.6192 0.4273 0.7368 0.034 Uiso 1 1 calc R . . C7 C 0.8051(3) 0.40078(15) 0.87312(15) 0.0260(6) Uani 1 1 d . . . C8 C 0.7405(3) 0.41698(16) 0.94964(16) 0.0316(6) Uani 1 1 d . . . H8A H 0.7326 0.4655 0.9669 0.038 Uiso 1 1 calc R . . C9 C 0.6875(4) 0.36292(18) 1.00111(18) 0.0416(8) Uani 1 1 d . . . H9A H 0.6441 0.3746 1.0532 0.050 Uiso 1 1 calc R . . C10 C 0.6979(4) 0.29271(18) 0.9767(2) 0.0472(9) Uani 1 1 d . . . H10A H 0.6622 0.2559 1.0122 0.057 Uiso 1 1 calc R . . C11 C 0.7600(4) 0.27566(18) 0.9009(2) 0.0461(8) Uani 1 1 d . . . H11A H 0.7661 0.2271 0.8839 0.055 Uiso 1 1 calc R . . C12 C 0.8136(4) 0.32900(15) 0.84928(18) 0.0355(7) Uani 1 1 d . . . H12A H 0.8565 0.3167 0.7972 0.043 Uiso 1 1 calc R . . C13 C 0.8203(3) 0.56335(14) 0.83019(16) 0.0265(6) Uani 1 1 d . . . C14 C 0.8944(4) 0.60060(16) 0.89510(17) 0.0357(7) Uani 1 1 d . . . H14A H 0.9784 0.5794 0.9224 0.043 Uiso 1 1 calc R . . C15 C 0.8477(5) 0.66780(17) 0.9203(2) 0.0485(9) Uani 1 1 d . . . H15A H 0.9004 0.6922 0.9640 0.058 Uiso 1 1 calc R . . C16 C 0.7252(4) 0.69940(17) 0.8822(2) 0.0476(9) Uani 1 1 d . . . H16A H 0.6920 0.7448 0.9008 0.057 Uiso 1 1 calc R . . C17 C 0.6508(4) 0.66486(17) 0.8169(2) 0.0459(8) Uani 1 1 d . . . H17A H 0.5677 0.6868 0.7895 0.055 Uiso 1 1 calc R . . C18 C 0.6989(3) 0.59772(16) 0.79170(19) 0.0358(7) Uani 1 1 d . . . H18A H 0.6474 0.5744 0.7467 0.043 Uiso 1 1 calc R . . C19 C 1.0887(3) 0.46966(14) 0.81210(15) 0.0244(6) Uani 1 1 d . . . C20 C 1.1789(3) 0.51145(16) 0.76107(17) 0.0321(7) Uani 1 1 d . . . H20A H 1.1354 0.5355 0.7140 0.039 Uiso 1 1 calc R . . C21 C 1.3294(3) 0.51867(18) 0.77751(19) 0.0389(7) Uani 1 1 d . . . H21A H 1.3882 0.5474 0.7419 0.047 Uiso 1 1 calc R . . C22 C 1.3948(3) 0.48400(17) 0.84601(18) 0.0350(7) Uani 1 1 d . . . H22A H 1.4981 0.4894 0.8577 0.042 Uiso 1 1 calc R . . C23 C 1.3095(3) 0.44161(16) 0.89728(18) 0.0340(7) Uani 1 1 d . . . H23A H 1.3541 0.4172 0.9438 0.041 Uiso 1 1 calc R . . C24 C 1.1573(3) 0.43486(14) 0.88034(16) 0.0284(6) Uani 1 1 d . . . H24A H 1.0990 0.4060 0.9160 0.034 Uiso 1 1 calc R . . O1TA O 0.7036(3) 0.30974(13) 0.28721(16) 0.0649(8) Uani 1 1 d . A . C1TA C 0.8021(5) 0.3018(2) 0.2204(2) 0.0579(10) Uani 1 1 d . . . H1TA H 0.8182 0.3473 0.1900 0.069 Uiso 0.436(9) 1 calc PR A 1 H1TB H 0.7697 0.2642 0.1802 0.069 Uiso 0.436(9) 1 calc PR A 1 H1TC H 0.7473 0.2797 0.1724 0.069 Uiso 0.564(9) 1 calc PR A 2 H1TD H 0.8339 0.3500 0.2024 0.069 Uiso 0.564(9) 1 calc PR A 2 C2TA C 0.9467(8) 0.2779(4) 0.2766(5) 0.035(2) Uiso 0.436(9) 1 d P A 1 H2TA H 1.0374 0.2724 0.2432 0.042 Uiso 0.436(9) 1 calc PR A 1 H2TB H 0.9660 0.3095 0.3257 0.042 Uiso 0.436(9) 1 calc PR A 1 C3TA C 0.8774(12) 0.2083(6) 0.2995(7) 0.070(3) Uiso 0.436(9) 1 d P A 1 H3TA H 0.9366 0.1809 0.3416 0.084 Uiso 0.436(9) 1 calc PR A 1 H3TB H 0.8516 0.1782 0.2501 0.084 Uiso 0.436(9) 1 calc PR A 1 C2TB C 0.9281(12) 0.2613(6) 0.2375(8) 0.097(3) Uiso 0.564(9) 1 d P A 2 H2TC H 1.0216 0.2882 0.2307 0.116 Uiso 0.564(9) 1 calc PR A 2 H2TD H 0.9304 0.2160 0.2054 0.116 Uiso 0.564(9) 1 calc PR A 2 C3TB C 0.8755(7) 0.2480(4) 0.3552(4) 0.047(2) Uiso 0.564(9) 1 d P A 2 H3TC H 0.9088 0.2013 0.3781 0.057 Uiso 0.564(9) 1 calc PR A 2 H3TD H 0.9121 0.2873 0.3920 0.057 Uiso 0.564(9) 1 calc PR A 2 C4TA C 0.7277(6) 0.2507(2) 0.3409(3) 0.0844(15) Uani 1 1 d . . . H4TA H 0.6398 0.2188 0.3408 0.101 Uiso 0.436(9) 1 calc PR A 1 H4TB H 0.7497 0.2666 0.3993 0.101 Uiso 0.436(9) 1 calc PR A 1 H4TC H 0.6749 0.2573 0.3943 0.101 Uiso 0.564(9) 1 calc PR A 2 H4TD H 0.6920 0.2061 0.3138 0.101 Uiso 0.564(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0198(2) 0.0283(2) 0.0229(2) 0.00064(15) 0.00165(14) -0.00203(16) Cl1 0.0307(4) 0.0296(4) 0.0234(3) -0.0013(3) 0.0042(3) -0.0020(3) Cl2 0.0384(4) 0.0332(4) 0.0330(4) 0.0016(3) 0.0034(3) 0.0087(3) Si1 0.0216(4) 0.0263(4) 0.0212(3) 0.0014(3) 0.0012(3) -0.0002(3) N1 0.0248(13) 0.0338(13) 0.0227(11) -0.0022(9) 0.0014(9) -0.0057(10) N2 0.0211(12) 0.0251(12) 0.0239(11) 0.0016(9) 0.0040(9) -0.0001(9) C1 0.0339(18) 0.052(2) 0.0270(14) -0.0050(13) 0.0001(12) -0.0106(15) C2 0.0360(19) 0.065(2) 0.0334(16) -0.0048(15) -0.0079(14) -0.0104(17) C3 0.0241(17) 0.055(2) 0.0441(17) -0.0089(15) -0.0071(13) -0.0047(15) C4 0.0227(16) 0.0468(19) 0.0370(16) -0.0090(13) 0.0045(12) -0.0024(14) C5 0.0232(15) 0.0284(14) 0.0271(13) -0.0029(11) 0.0022(11) -0.0016(12) C6 0.0251(15) 0.0338(16) 0.0254(13) -0.0016(11) 0.0053(11) -0.0019(12) C7 0.0213(15) 0.0339(16) 0.0226(13) 0.0031(11) -0.0011(10) 0.0017(12) C8 0.0333(17) 0.0371(16) 0.0244(14) 0.0016(12) 0.0007(12) -0.0013(13) C9 0.0400(19) 0.056(2) 0.0287(15) 0.0122(14) 0.0062(13) -0.0023(16) C10 0.048(2) 0.044(2) 0.0498(19) 0.0225(16) 0.0028(16) -0.0072(16) C11 0.053(2) 0.0309(17) 0.054(2) 0.0099(15) 0.0047(17) 0.0001(16) C12 0.0406(19) 0.0299(16) 0.0362(16) 0.0019(12) 0.0071(13) 0.0013(14) C13 0.0239(15) 0.0294(15) 0.0264(13) 0.0050(11) 0.0053(11) -0.0022(12) C14 0.0423(19) 0.0346(17) 0.0301(15) -0.0012(13) -0.0013(13) 0.0066(14) C15 0.073(3) 0.0373(19) 0.0347(17) -0.0064(14) 0.0038(16) 0.0061(18) C16 0.061(2) 0.0293(17) 0.054(2) 0.0017(15) 0.0157(17) 0.0102(16) C17 0.0324(19) 0.0342(18) 0.071(2) 0.0103(16) 0.0051(16) 0.0076(14) C18 0.0258(17) 0.0327(17) 0.0489(18) 0.0027(13) -0.0015(13) 0.0002(13) C19 0.0225(14) 0.0266(14) 0.0239(13) -0.0042(11) -0.0013(10) 0.0024(12) C20 0.0275(16) 0.0399(17) 0.0288(14) 0.0040(12) -0.0035(11) -0.0006(13) C21 0.0258(17) 0.0498(19) 0.0411(17) 0.0071(14) 0.0013(13) -0.0038(14) C22 0.0199(15) 0.0462(19) 0.0386(16) -0.0084(14) -0.0050(12) 0.0042(13) C23 0.0325(17) 0.0386(17) 0.0305(15) -0.0029(13) -0.0059(12) 0.0083(14) C24 0.0284(16) 0.0298(15) 0.0270(13) 0.0000(11) -0.0011(11) 0.0004(12) O1TA 0.084(2) 0.0443(15) 0.0665(16) 0.0118(12) 0.0166(15) 0.0104(14) C1TA 0.073(3) 0.052(2) 0.048(2) -0.0014(17) 0.0001(19) -0.006(2) C4TA 0.130(5) 0.052(3) 0.073(3) 0.017(2) 0.024(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.130(2) . ? Fe1 N2 2.217(2) . ? Fe1 Cl2 2.2640(8) . ? Fe1 Cl1 2.3727(8) . ? Fe1 Cl1 2.5353(7) 3_766 ? Cl1 Fe1 2.5353(7) 3_766 ? Si1 N2 1.789(2) . ? Si1 C19 1.854(3) . ? Si1 C13 1.868(3) . ? Si1 C7 1.872(3) . ? N1 C1 1.335(3) . ? N1 C5 1.357(3) . ? N2 C6 1.276(4) . ? C1 C2 1.391(4) . ? C2 C3 1.376(4) . ? C3 C4 1.383(4) . ? C4 C5 1.383(4) . ? C5 C6 1.472(4) . ? C7 C8 1.394(4) . ? C7 C12 1.397(4) . ? C8 C9 1.392(4) . ? C9 C10 1.373(5) . ? C10 C11 1.377(5) . ? C11 C12 1.386(4) . ? C13 C18 1.397(4) . ? C13 C14 1.402(4) . ? C14 C15 1.387(4) . ? C15 C16 1.379(5) . ? C16 C17 1.384(5) . ? C17 C18 1.390(4) . ? C19 C24 1.397(4) . ? C19 C20 1.399(4) . ? C20 C21 1.381(4) . ? C21 C22 1.387(4) . ? C22 C23 1.382(4) . ? C23 C24 1.396(4) . ? O1TA C1TA 1.407(5) . ? O1TA C4TA 1.410(4) . ? C1TA C2TB 1.386(10) . ? C1TA C2TA 1.625(9) . ? C2TA C3TA 1.492(12) . ? C3TA C4TA 1.708(11) . ? C2TB C3TB 1.956(13) . ? C3TB C4TA 1.346(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 77.68(8) . . ? N1 Fe1 Cl2 116.57(7) . . ? N2 Fe1 Cl2 91.77(6) . . ? N1 Fe1 Cl1 106.91(7) . . ? N2 Fe1 Cl1 92.06(6) . . ? Cl2 Fe1 Cl1 136.15(3) . . ? N1 Fe1 Cl1 94.20(6) . 3_766 ? N2 Fe1 Cl1 170.98(6) . 3_766 ? Cl2 Fe1 Cl1 95.42(3) . 3_766 ? Cl1 Fe1 Cl1 86.53(2) . 3_766 ? Fe1 Cl1 Fe1 93.47(2) . 3_766 ? N2 Si1 C19 113.11(11) . . ? N2 Si1 C13 107.52(11) . . ? C19 Si1 C13 107.64(12) . . ? N2 Si1 C7 106.35(11) . . ? C19 Si1 C7 109.26(12) . . ? C13 Si1 C7 113.06(12) . . ? C1 N1 C5 117.5(2) . . ? C1 N1 Fe1 128.16(19) . . ? C5 N1 Fe1 114.30(17) . . ? C6 N2 Si1 118.90(18) . . ? C6 N2 Fe1 110.49(17) . . ? Si1 N2 Fe1 129.99(12) . . ? N1 C1 C2 122.7(3) . . ? C3 C2 C1 119.3(3) . . ? C2 C3 C4 118.9(3) . . ? C3 C4 C5 118.8(3) . . ? N1 C5 C4 122.8(2) . . ? N1 C5 C6 115.0(2) . . ? C4 C5 C6 122.2(2) . . ? N2 C6 C5 121.9(2) . . ? C8 C7 C12 118.2(3) . . ? C8 C7 Si1 122.4(2) . . ? C12 C7 Si1 119.4(2) . . ? C7 C8 C9 120.7(3) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 120.4(3) . . ? C11 C12 C7 120.6(3) . . ? C18 C13 C14 116.7(3) . . ? C18 C13 Si1 124.1(2) . . ? C14 C13 Si1 119.2(2) . . ? C15 C14 C13 121.3(3) . . ? C16 C15 C14 120.4(3) . . ? C15 C16 C17 119.9(3) . . ? C16 C17 C18 119.3(3) . . ? C17 C18 C13 122.4(3) . . ? C24 C19 C20 117.3(2) . . ? C24 C19 Si1 119.4(2) . . ? C20 C19 Si1 122.5(2) . . ? C21 C20 C19 121.6(3) . . ? C20 C21 C22 120.0(3) . . ? C23 C22 C21 120.0(3) . . ? C22 C23 C24 119.6(3) . . ? C19 C24 C23 121.5(3) . . ? C1TA O1TA C4TA 106.5(3) . . ? C2TB C1TA O1TA 115.8(5) . . ? C2TB C1TA C2TA 25.8(5) . . ? O1TA C1TA C2TA 97.1(4) . . ? C3TA C2TA C1TA 92.3(6) . . ? C2TA C3TA C4TA 91.6(7) . . ? C1TA C2TB C3TB 92.5(6) . . ? C4TA C3TB C2TB 95.3(5) . . ? C3TB C4TA O1TA 105.7(5) . . ? C3TB C4TA C3TA 42.4(4) . . ? O1TA C4TA C3TA 104.0(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.555 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.074 #==== END data_FO3617 _database_code_depnum_ccdc_archive 'CCDC 736366' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Fe N4 Si2' _chemical_formula_sum 'C48 H42 Fe N4 Si2' _chemical_formula_weight 786.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.4134(8) _cell_length_b 37.3593(16) _cell_length_c 9.6921(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8115.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 14135 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14135 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4559 _reflns_number_gt 3281 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(17) _refine_ls_number_reflns 4559 _refine_ls_number_parameters 249 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.2500 0.2500 0.59943(6) 0.02509(15) Uani 1 2 d S . . Si1 Si 0.13182(3) 0.27770(2) 0.44490(8) 0.02447(19) Uani 1 1 d . . . N1 N 0.27612(9) 0.29126(6) 0.7356(3) 0.0287(6) Uani 1 1 d . . . N2 N 0.19416(9) 0.28711(6) 0.5356(2) 0.0250(5) Uani 1 1 d . . . C1 C 0.31482(12) 0.28985(8) 0.8421(4) 0.0399(8) Uani 1 1 d . . . H1A H 0.3287 0.2671 0.8717 0.048 Uiso 1 1 calc R . . C2 C 0.33509(13) 0.31966(9) 0.9093(4) 0.0474(9) Uani 1 1 d . . . H2A H 0.3619 0.3177 0.9848 0.057 Uiso 1 1 calc R . . C3 C 0.31543(12) 0.35278(9) 0.8644(4) 0.0458(9) Uani 1 1 d . . . H3A H 0.3294 0.3740 0.9073 0.055 Uiso 1 1 calc R . . C4 C 0.27533(12) 0.35459(8) 0.7570(3) 0.0349(7) Uani 1 1 d . . . H4A H 0.2616 0.3772 0.7252 0.042 Uiso 1 1 calc R . . C5 C 0.25515(10) 0.32342(7) 0.6956(3) 0.0259(6) Uani 1 1 d . . . C6 C 0.21084(11) 0.32308(7) 0.5787(3) 0.0281(7) Uani 1 1 d . . . H6A H 0.1745 0.3361 0.6076 0.034 Uiso 1 1 calc R . . H6B H 0.2282 0.3359 0.4989 0.034 Uiso 1 1 calc R . . C7 C 0.12162(11) 0.22762(7) 0.4587(3) 0.0280(7) Uani 1 1 d . . . C8 C 0.08681(13) 0.21124(8) 0.5585(3) 0.0385(8) Uani 1 1 d . . . H8A H 0.0624 0.2256 0.6162 0.046 Uiso 1 1 calc R . . C9 C 0.08662(15) 0.17447(9) 0.5767(4) 0.0520(10) Uani 1 1 d . . . H9A H 0.0633 0.1639 0.6477 0.062 Uiso 1 1 calc R . . C10 C 0.12071(16) 0.15333(9) 0.4906(4) 0.0562(11) Uani 1 1 d . . . H10A H 0.1208 0.1281 0.5030 0.067 Uiso 1 1 calc R . . C11 C 0.15438(14) 0.16817(9) 0.3876(4) 0.0501(11) Uani 1 1 d . . . H11A H 0.1773 0.1534 0.3280 0.060 Uiso 1 1 calc R . . C12 C 0.15475(12) 0.20548(8) 0.3709(4) 0.0370(8) Uani 1 1 d . . . H12A H 0.1778 0.2159 0.2990 0.044 Uiso 1 1 calc R . . C13 C 0.06484(11) 0.30259(7) 0.5142(3) 0.0259(7) Uani 1 1 d . . . C14 C 0.03098(11) 0.32579(7) 0.4339(4) 0.0344(7) Uani 1 1 d . . . H14A H 0.0407 0.3286 0.3391 0.041 Uiso 1 1 calc R . . C15 C -0.01678(12) 0.34508(8) 0.4883(4) 0.0400(8) Uani 1 1 d . . . H15A H -0.0387 0.3610 0.4311 0.048 Uiso 1 1 calc R . . C16 C -0.03208(13) 0.34103(8) 0.6240(4) 0.0406(9) Uani 1 1 d . . . H16A H -0.0649 0.3540 0.6609 0.049 Uiso 1 1 calc R . . C17 C 0.00007(12) 0.31810(8) 0.7077(4) 0.0405(8) Uani 1 1 d . . . H17A H -0.0108 0.3150 0.8017 0.049 Uiso 1 1 calc R . . C18 C 0.04829(12) 0.29978(8) 0.6528(3) 0.0326(7) Uani 1 1 d . . . H18A H 0.0710 0.2847 0.7117 0.039 Uiso 1 1 calc R . . C19 C 0.13482(12) 0.28847(7) 0.2554(3) 0.0278(7) Uani 1 1 d . . . C20 C 0.18078(12) 0.30877(8) 0.1978(4) 0.0358(7) Uani 1 1 d . . . H20A H 0.2124 0.3169 0.2552 0.043 Uiso 1 1 calc R . . C21 C 0.18128(15) 0.31731(9) 0.0586(3) 0.0447(9) Uani 1 1 d . . . H21A H 0.2127 0.3316 0.0225 0.054 Uiso 1 1 calc R . . C22 C 0.13685(14) 0.30544(9) -0.0279(3) 0.0426(8) Uani 1 1 d . . . H22A H 0.1376 0.3112 -0.1234 0.051 Uiso 1 1 calc R . . C23 C 0.09118(15) 0.28506(9) 0.0259(4) 0.0452(9) Uani 1 1 d . . . H23A H 0.0601 0.2768 -0.0326 0.054 Uiso 1 1 calc R . . C24 C 0.09050(12) 0.27660(9) 0.1640(3) 0.0374(8) Uani 1 1 d . . . H24A H 0.0589 0.2622 0.1987 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0250(2) 0.0230(3) 0.0272(3) 0.000 0.000 0.0039(3) Si1 0.0229(4) 0.0277(4) 0.0227(5) 0.0014(3) -0.0013(3) 0.0014(3) N1 0.0246(12) 0.0331(13) 0.0285(16) 0.0012(11) -0.0021(11) 0.0014(10) N2 0.0217(11) 0.0229(11) 0.0303(15) -0.0028(10) -0.0019(10) 0.0000(10) C1 0.0349(15) 0.0497(18) 0.035(2) -0.0020(18) -0.0092(17) -0.0001(14) C2 0.0377(17) 0.065(2) 0.040(2) -0.0129(18) -0.0081(16) -0.0079(17) C3 0.0374(17) 0.055(2) 0.045(2) -0.0237(19) 0.0084(17) -0.0175(16) C4 0.0345(15) 0.0298(16) 0.040(2) -0.0078(15) 0.0072(15) -0.0068(13) C5 0.0213(13) 0.0291(15) 0.0273(18) -0.0043(13) 0.0060(13) -0.0013(11) C6 0.0260(13) 0.0257(15) 0.033(2) 0.0002(14) -0.0036(14) 0.0043(12) C7 0.0247(13) 0.0329(15) 0.0265(18) 0.0009(14) -0.0090(13) -0.0041(12) C8 0.0394(17) 0.0400(17) 0.036(2) 0.0033(15) -0.0089(15) -0.0108(14) C9 0.063(2) 0.0416(19) 0.051(3) 0.011(2) -0.022(2) -0.0223(17) C10 0.064(2) 0.0312(19) 0.073(3) 0.003(2) -0.041(2) -0.0115(18) C11 0.0438(19) 0.0377(18) 0.069(3) -0.0138(19) -0.0253(19) 0.0083(16) C12 0.0306(15) 0.0359(16) 0.044(2) -0.0064(16) -0.0098(16) 0.0048(13) C13 0.0254(14) 0.0277(15) 0.0248(18) -0.0011(13) -0.0032(13) -0.0037(12) C14 0.0302(14) 0.0386(16) 0.034(2) 0.0064(15) -0.0009(14) 0.0070(13) C15 0.0317(16) 0.0441(19) 0.044(2) -0.0012(17) -0.0023(15) 0.0067(14) C16 0.0281(15) 0.0415(18) 0.052(3) -0.0161(17) 0.0042(16) -0.0012(14) C17 0.0403(17) 0.0497(19) 0.032(2) -0.0094(16) 0.0069(16) -0.0080(15) C18 0.0346(15) 0.0396(17) 0.0234(19) -0.0041(13) -0.0015(13) 0.0033(14) C19 0.0255(14) 0.0284(14) 0.0297(19) 0.0015(14) 0.0019(13) 0.0026(12) C20 0.0324(15) 0.0440(18) 0.031(2) -0.0007(16) -0.0019(15) -0.0020(14) C21 0.051(2) 0.053(2) 0.031(2) 0.0069(16) 0.0105(16) -0.0128(16) C22 0.057(2) 0.054(2) 0.0167(19) 0.0062(15) 0.0041(16) -0.0020(17) C23 0.0468(19) 0.060(2) 0.029(2) 0.0004(18) -0.0059(16) -0.0033(17) C24 0.0298(15) 0.053(2) 0.029(2) 0.0035(16) 0.0001(14) -0.0082(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.967(2) 14 ? Fe1 N2 1.967(2) . ? Fe1 N1 2.112(2) 14 ? Fe1 N1 2.112(2) . ? Si1 N2 1.688(2) . ? Si1 C19 1.881(3) . ? Si1 C7 1.890(3) . ? Si1 C13 1.889(3) . ? N1 C5 1.347(3) . ? N1 C1 1.349(4) . ? N2 C6 1.456(3) . ? C1 C2 1.368(4) . ? C2 C3 1.384(5) . ? C3 C4 1.377(4) . ? C4 C5 1.384(4) . ? C5 C6 1.507(4) . ? C7 C8 1.385(4) . ? C7 C12 1.400(4) . ? C8 C9 1.385(4) . ? C9 C10 1.380(5) . ? C10 C11 1.369(5) . ? C11 C12 1.404(4) . ? C13 C14 1.390(4) . ? C13 C18 1.398(4) . ? C14 C15 1.394(4) . ? C15 C16 1.368(5) . ? C16 C17 1.382(4) . ? C17 C18 1.386(4) . ? C19 C20 1.396(4) . ? C19 C24 1.403(4) . ? C20 C21 1.386(5) . ? C21 C22 1.376(4) . ? C22 C23 1.378(4) . ? C23 C24 1.376(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 N2 Fe1 N2 143.37(14) 14 . ? N2 Fe1 N1 81.86(9) 14 14 ? N2 Fe1 N1 122.30(9) . 14 ? N2 Fe1 N1 122.30(9) 14 . ? N2 Fe1 N1 81.86(9) . . ? N1 Fe1 N1 102.65(13) 14 . ? N2 Si1 C19 115.76(13) . . ? N2 Si1 C7 105.63(11) . . ? C19 Si1 C7 106.58(13) . . ? N2 Si1 C13 111.72(12) . . ? C19 Si1 C13 105.67(13) . . ? C7 Si1 C13 111.46(12) . . ? C5 N1 C1 118.7(3) . . ? C5 N1 Fe1 111.97(19) . . ? C1 N1 Fe1 128.9(2) . . ? C6 N2 Si1 123.65(17) . . ? C6 N2 Fe1 113.39(16) . . ? Si1 N2 Fe1 122.93(12) . . ? N1 C1 C2 123.1(3) . . ? C1 C2 C3 118.2(3) . . ? C4 C3 C2 119.3(3) . . ? C3 C4 C5 119.8(3) . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C6 116.1(2) . . ? C4 C5 C6 123.1(3) . . ? N2 C6 C5 113.1(2) . . ? C8 C7 C12 117.5(3) . . ? C8 C7 Si1 123.7(2) . . ? C12 C7 Si1 118.5(2) . . ? C7 C8 C9 121.9(3) . . ? C10 C9 C8 119.3(3) . . ? C11 C10 C9 121.0(3) . . ? C10 C11 C12 119.3(3) . . ? C7 C12 C11 120.9(3) . . ? C14 C13 C18 116.1(3) . . ? C14 C13 Si1 122.8(2) . . ? C18 C13 Si1 121.0(2) . . ? C15 C14 C13 122.0(3) . . ? C16 C15 C14 119.9(3) . . ? C15 C16 C17 120.1(3) . . ? C16 C17 C18 119.2(3) . . ? C17 C18 C13 122.6(3) . . ? C20 C19 C24 116.2(3) . . ? C20 C19 Si1 122.2(2) . . ? C24 C19 Si1 121.6(2) . . ? C19 C20 C21 121.4(3) . . ? C22 C21 C20 120.9(3) . . ? C23 C22 C21 119.0(3) . . ? C22 C23 C24 120.2(3) . . ? C23 C24 C19 122.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.271 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.056